TW201221521A - An improved process for preparation of trialkyl phosphites - Google Patents

Abstract

According to an aspect of the invention, there is provided an improved process for the preparation of trialkyl phosphite of Formula I: said process comprising reacting trialkyl phosphite of Formula II with alkanol of formula III R<SP>1</SP>-OH III such that R<SP>1</SP> represents an alkyl moiety having 8 to 16 carbon atoms and R represents an alkyl moiety having 1 to 3 carbon atoms. Also disclosed is the compound of formula I that is substantially free of a phenolic impurity.

Description

201221521 VI. Description of the Invention: [Technical Field of the Invention] [0001] The present invention relates to an improved method for producing a trialkyl phosphite, and to a tristeamidate produced therefrom. [Prior Art] [0002] Various uses of trialkyl phosphites have been reported in the art, for example, as additives for synthetic resins, lubricants, defoamers, and for the manufacture of various chemicals. The use of stabilizers such as intermediates and the like. A number of methods have been developed for the preparation of trialkyl phosphites. For example, triethyl phosphite is prepared by the reaction of tri-phosphorus phosphorus with ethanol in the presence of a hydrogen chloride acceptor such as an amine or an amine. However, when triethyl phosphite is prepared by this technique, various problems are associated. For example, the reaction is highly exothermic and therefore expensive cooling equipment must be used to control the reaction temperature. The product formed is not obtained in pure form, so a lengthy procedure that is not economically feasible is used to obtain a pure product. More recently, trialkyl phosphites have been prepared by transesterification of triaryl phosphites such as triphenyl phosphite with alkyl alcohols in the presence of a basic catalyst. However, when this technique is applied to a lower alkyl alcohol (e.g., ethanol), it is not easy to obtain separation of the trialkyl methacrylate (e.g., triethyl phosphite) from other reaction products. The product needs to be separated from the reaction mixture by a tedious and cumbersome procedure. In addition, it has been found that the trialkyl phosphite prepared by this method always includes 0.1% to 0.3% or more of phenolic impurities, and due to its inherent Qin nature, the use of the mixed impurities for its intended use. It is not wanted. There is a need in the art to produce a dialkyl phosphite that is substantially free of phenolic impurities. 100134551^Single number A〇101 帛4 pages/total 29 pages 1013064654-0 201221521 The need for the method. Gu Yu "substantially no" in this article is intended to mean that there is no bribe impurity or contains more than 1QQ _ impurities. This secret impurity is derived from the aryl moiety of the triaryl sulphate starting material and is highly undesirable. Accordingly, it is clear in the art that there is a need for a trialkyl group which is substantially free of secret impurities and a method for preparing the same. U.S. Patent No. 3,636,145 discloses the preparation of a process for the preparation of a triallyl phosphite by a transesterification reaction involving tridecyl phosphite and an enol. According to the claimed process, an essential element of the disclosed invention is the presence of a basic catalyst and the presence of a non-azeotropic solvent in the process. U.S. Patent No. 3,184,496 discloses the preparation and recovery of trimethyl linoleate and the preparation of trimethyl phosphite derivatives. This method also discloses the use of a basic catalyst in the reaction. The above method of Φξ: and is involved in lengthy and tedious work processes to obtain pure products, or the use of catalysts and solvents, thus making these methods uneconomical and less environmentally friendly. There is therefore a need in the art to develop an environmentally friendly, efficient and economical process for the manufacture of trialkyl phosphites without the use of any solvents and/or basic catalysts to obtain the product in high yields and purity. OBJECT OF THE INVENTION One object of the present invention is to provide an improved process for the preparation of trialkyl phosphite compounds. Another object of the present invention is to provide an improved process for the preparation of trialkyl phosphites in high yields and wall fractions using a percentage. Another object of the present invention is to provide an improved process for the preparation of trialkyl phosphites. The improved process is environmentally friendly. 1013064654-0 10013455 Production Order No. AOm Page 5 of 29 201221521 Another aspect of the present invention provides an improved method for preparing trisperate. The improved method is economically feasible and less time consuming. . Still another object of the present invention is to provide an improved process which results in the preparation of trialkyl phosphites which are substantially free of impurities. The present invention (4) - a catalogue provides a trialkyl phosphite which is read without _f or contains less than 100 ppm of phenolic impurities. These and other objects of the invention will become apparent from the following detailed description. SUMMARY OF THE INVENTION [0003] According to an aspect of the invention, there is provided an improved method for preparing a molecular formula phosphite:

R ο.

R b

-〇——R-type sub-segment will contain the method of inclusion

R salt phosphorus subunit alkane

R Io / \o - RP and the alkanol rLoH of the formula 111 are produced by the reaction number No. A0101 * 6 pages / 29 pages III201221521, such that Rl represents an alkyl moiety having 8 to 16 carbon atoms, and R Represents an alkyl moiety having from 1 to 3 carbon atoms. In another aspect, there is provided a trialkyl phosphite compound of the formula:

R ο / \olhR I P I1 \o R such that rI represents an alkyl moiety having 8 to 16 carbon atoms, wherein the compound of formula I is substantially free of phenolic impurities. [Embodiment] The present invention provides an improved process for the preparation of a trialkyl phosphite of formula I by reacting a trialkyl phosphite of formula II with an alkanol of formula III as described above, wherein R1 represents an alkyl moiety having (^-(:1(: carbon atom), and R represents an alkyl moiety having \-(:3 carbon atoms). The reaction is represented in the following schematic form. It is not desired to be limited by theory. It is generally believed that the reaction may continue via the intermediate monoalkyl phosphite and dialkyl phosphite to produce the tripent phosphite compound of formula I. Reaction pathway of phosphite 10013455^^^ A〇101 Page 7 of 29 1〇13〇64654-〇201221521 3 -OH Alkanol molecular formula Trialkylphosphonium ruthenium (OR) 3P _ Molecular Formula 1 _ Section 1

0-R

0-P

R monoalkyl phosphite intermediate I

R 〇-'R \ / 0—P 0I, R dihistyl (tetra) acid gold intermediate H

0-R

0-P

R trialkyl δ phosphoric acid S △ » C - 210 C 喑 segment 11

3R - ΟΗ IV

0-R 0 —Ρ Trialkyl phosphite Formula 1 According to one aspect, the present invention relates to the preparation of the formula I by reacting a trialkyl phosphite of the formula π with an alkanol of the formula oxime as described above. An improved process for the anhydride acidate wherein the reaction is carried out in the absence of a catalyst and/or solvent. In a specific embodiment, the improved process of the present invention comprises reacting the trialkyl phosphite of the formula with the alkyl alcohol in the absence or absence of a solvent or in the absence of a catalytic hydrazine and a solvent. . In a specific real scarf, the molecular illusion of the genus phosphazone _# r is selected from carbon bonds in the range of c8-c16, preferably c9-c15 and more preferably C10~Ci3. In a specific embodiment, the 'molecular formula m' is selected from the group consisting of alkanols having a carbon bond range of C8'c16, preferably c9-c15 and more preferably (10-〇13). Page 8 of 29 Single No. A0101 1013064654-0 201221521 In a further embodiment, the R group in the trialkyl phosphite of the formula II is selected from the group consisting of an alkyl moiety having a Ci-C3 carbon atom, and R is preferably a methyl group. According to a specific embodiment, the trialkyl phosphite of formula II is added to the alkanol of formula III at a temperature ranging from 75 ° C to 180 ° C. In yet another embodiment, The trialkyl phosphite of the formula II is added to the alkanol of the formula III and stirred for 5-7 hours. In a further embodiment, the alkylalkanol of the formula is related to the trialkyl group of the formula II The phosphite is in a molar ratio of 5:3:1, preferably in a ratio of 4: 1. In another embodiment, after the addition of the trialkyl phosphite, the reaction mass is heated to a temperature between 180 ° C and 220 ° C. The reaction mass is maintained at this temperature to allow the reaction to be complete. In a specific embodiment, the reaction mass is maintained between about 18 Torr. between C-220X and maintained at this temperature for a period of about 2-4 hours. It has been found that the reaction mass is maintained at The elevated temperature results in an increase in the yield of the target product. In one embodiment, the foregoing reaction mass is maintained for a period of 2-4 hours of the elevated temperature of at least the alcoholic by-product of the formula 丨7 produced during the reaction. Above the boiling point of R-0H, it has been found that maintaining the temperature of the reaction mass above at least the boiling point of the alcohol by-product results in simultaneous removal of the by-product from the reaction system, which has been found to increase the product of the formula The yield of 1013064654-0 10013455, the production number Α〇101 帛9 pages/total 29 pages 201221521 Therefore, the specific embodiment of the towel, in the reaction class, the molecular formula produced _ Simultaneous removal of the alcohol. The alcohol by-product is more robust by condensation and is cooled by condensing it at a lower X temperature without allowing the alcohol to leave the system. Excellent The method makes the method cost-effective and environmentally safe. Therefore, in this specific case, the bribe is provided by an improved method for preparing the trialkyl phosphite of formula I: &lt; 0-R1 〇一Ρ \ 〇 The method comprises: (a) adding a compound of formula π to the rider's third wire by means of a temperature between 75H8CTC

Ro—/p, o—RI\o R is reacted with the alcoholic alcohol rl〇h of the formula III such that R1 represents a thiol moiety having 8 to 16 carbon atoms, and the digraph has (5) 100134551*^ A〇101 10 pages/total 29 pages 1013064654-0 201221521 alkyl moiety of carbon atom; (b) maintaining the reaction mass synchronously shifting over the boiling temperature of the alkanol having at least 1 to 3 carbon atoms for a predetermined period of time Except for the alcoholic by-product R-〇H of the formula IV produced during the reaction; and (c) recovering the target compound of the formula I by filtration; wherein the improvement is contained in the absence of a catalyst or lack of a solvent or lack of a catalyst and a solvent The trialkyl phosphite of the formula is reacted with the alkanol. In a specific embodiment, after completion of step (b) above, the reaction mass is cooled under a blunt gas. The preferred inert gas is nitrogen. The cooled reaction mass was subjected to a vacuum at 80-100 DC to remove any residue of the alcohol by-product. In one embodiment, the reaction mass is again heated to ig 〇 2Q [|DC for a sufficient period of time under 1-2 vacuum to remove any remaining traces of alcohol. In a specific embodiment, the reaction is thereafter cooled, preferably cooled to a temperature of about 40 ° C, and the target compound is recovered by filtration. Thus, in another embodiment, the invention provides an improved process for the preparation of a trialkyl phosphite of formula I: Ό-R1 0 - p \ 〇 I,

R Page 11 of 29 10013455 Production · Single Number A0101 201221521 The method comprises: (a) by slowly bringing the compound of formula II at a temperature between 75 ° C &quot; 18 (TC) for at least 0.5 hours Addition to the sterol RLOH of the formula in, and after the addition of the compound of the formula II to the aniolate, the tribasic acid ylide of the formula II

〇-R is reacted with an alkanol F^-OH of formula III such that p 1 represents an alkyl moiety having 8 to 16 carbon atoms, and R represents an alkyl moiety having 1 to 3 carbon atoms, b) maintaining the temperature of the reaction mass at a boiling point of the alkanol having at least 1 to 3 carbon atoms for a predetermined period of time while synchronously removing the alcohol by-product R-0H produced during the reaction; (c) Optionally, cooling the reaction product under blunt gas; (d) heating the cooled reaction product to 19D_2GD0C under a vacuum pressure of 1-2 legs for a sufficient period of time; and (e) cooling the reaction product to about 400C The temperature, and the recovery of the compound of formula I; wherein the modification comprises reacting the trialkyl sulfite of formula II with the animate in the absence or absence of a solvent or a lack of a catalyst and a solvent. 10013455^^'^^ A0101 Page 12 of 29 1013064654-0 201221521 In a further embodiment, at approximately 75. 〇180. (The trialkyl phosphite of formula II is added to the oleanol of the formula ' at the elevated temperature of '', optionally maintained at the same temperature for 〇6 hours, and then the reaction temperature is raised to about 195 °C-21 (TC 'and at about the same temperature for about 2-4 hours' to obtain the desired trialkyl phosphite of formula I in high yield and purity. In yet another embodiment 'In 3-7 hours' at 17 〇. Trimethyl sulphate was added to the alcohol at 〇180 C, followed by 丨95. (;-21 〇 C disturbed for about 2-4 hours. In a particular embodiment, the product is isolated by methods known in the art. In a particular embodiment, the trialkyl phosphite of formula I is obtained in more than 85% yield. The process described is completely solvent free and catalyst free, which makes the process environmentally friendly. It has been surprisingly found that in the absence of solvents and/or catalysts compared to conventional processes using catalysts and/or solvents , the target compound of formula I is surprisingly higher yield Thus, it has been surprisingly found that in the absence of catalyst and/or lysing, the percentage of utilization of the initial phosphorus content derived from the starting trialkyl phosphite is maximized. Therefore, the present method is completely old. Use of the starting reactant having a silk moiety "The inventors have found that the elimination of a starting material having an aryl moiety results in the formation of a trisyl sub-salt compound which is substantially free of phenolic impurities. Thus, in this regard, The present invention provides a trialkyl phosphite compound of the formula :: bundle number A0101 10013455 wide page 13 / total 29 page 1013064654-0 201221521

1-R ί 1 I ο / \OIR p I \o R , such that Ri represents a aryl moiety having 8 to 16 carbon atoms wherein the compound of formula I is substantially free of _impurities. The phrase "substantially absent" is intended herein to mean that the tricarboyl sulphate is completely free of secret impurities or contains less than 1 〇〇 _ of the desired impurities. The term "secret impurity" means all compounds which may be derived from the test and/or include an acid-substituting compound which is substituted with a benzene ring or more highly substituted than the starting triaryl sulfonate compound. Specific embodiments of the invention are explained in the table below. The following examples are presented to more fully define the invention without any intent. All percentages and ratios are by weight to weight ratio unless otherwise specifically stated. Example 1 Preparation of triisodecyl oxalate in the presence of sodium sterol. In a clean dry reaction flask, 316 g of isodecyl alcohol was added under n2 gas and allowed to mix for 5 minutes. Then add 45 gm of sodium methoxide and stir. The temperature was then raised to 75. 0 and then 63 qing of trimethyl phosphite was added to isodecyl alcohol while maintaining the temperature. The reaction temperature was then raised to 195-20 ITC and the reaction mass was stirred at the same temperature for 2 hours. During the process, methanol 10013455 produced as a by-product number A0101, page I4, page 29, 1013064654-0, 201221521 was simultaneously removed. The reaction mass was cooled to 8 〇 - 10 ° C under N 2 gas while a vacuum was applied to recover the isodecyl alcohol. The reaction mass was then maintained at 190-200 ° C under vacuum to remove traces of isodecyl alcohol. This temperature was then allowed to reach 4 ° C under N2 and the product was recovered after filtration. Yield of the product: 82.47% Phenolic content: NIL Example 2 Triisodecyl phosphite was prepared without using sodium decoxide. In a clean dry reaction flask, 316 gra of isodecyl alcohol was added under N2 gas and stirred for 5 minutes" and then the temperature was raised to 75 °C. Then, 63 gm of trimethyl phosphite was added to isodecyl alcohol in 0.5 hour while maintaining the temperature. The reaction temperature was then raised to 195-20 (TC) and the reaction mass was scrambled for 2 hours at the same temperature. During this process, the sterol produced as a by-product was removed simultaneously. Cool down to 80-100 ° C ' while applying vacuum to recover the isodecyl alcohol' and then maintain the reaction mass at 190-20 (TC) under 1-2 ram vacuum to remove traces of isodecyl alcohol. The temperature was then allowed to reach 40. 0 under |S|2 and the product was recovered after filtration. Yield of the product: 93.82% Phenolic content: NIL Example 3 Preparation of triisodecyl phosphite: in a clean In the dry reactor, add 2743 Kg of isodecyl alcohol 1013064654-0 under 1⁄2 gas and mix for 5 minutes. Then raise the temperature to 95 ° C. Then the temperature is 10013455. Page / Total 29 pages 201221521 Maintained at a temperature between 95-98 ° C, then add 542 Kg of sub-acid trimethyl vinegar to isodecyl alcohol (total addition time 5 hours). Then raise the reaction temperature to 19 {TC-20 (TC, and the reaction material was mixed at the same temperature for 2 hours. During the method, as The sterol produced by the product is simultaneously removed and recovered by condensation. The reaction mass is cooled to 80-l 〇 (rc ' while applying a vacuum to recover the trace amount of alcohol. Then at 1- The 2 mm true reaction material was transferred to (10) - 2 Torr C to remove the last trace of isodecyl alcohol. The temperature was then allowed to come to 40 C under the helium and the product was recovered after filtration. Yield: 92% Specific gravity at 25 ° C: 〇.88~〇9 阳 Refractive index at 25 ° C: 145 ~ 丨 46 〇 phenolic content: NIL Also used in the above examples 1-3 Method for the following example Table 1 1〇〇13455 Production Order No. A0101 [0005]

Page 16 of 29 Reactive Columns Recovered Yield gm of Alkanol (%) in 5 hours 1,1 —---sterol-90 --- — _ 474 in gm ; (94.42) 95-100 Isodecyl alcohol °C plus -179 into TMP; gm at 195-207 pages --- 1013064654-0 201221521

Stir at °C for 2 hours. 2 TMP; isodecyl alcohol in 70-80 methanol-90 471 125; 632 〇c added to gm; (93.82) TMP; isopropanol mixed 0. 5 small -179 hours; stirred at gm 195-207 °C for 2 hours . 3 TMP; isodecyl alcohol in 70-80 methanol - 82 472 125 ; 632 . (: Add gm; (94) TMP; stir isopropanol to mix 9.5 min -181; stir at gm 195-207 °C for 2 hours. 4 TMP; isotritate in methanol-95 583 125 ani alcohol; -140 gm ; (92. 83) 800 X added isotritium TMP, stir-fry alcohol for 3 hours -237 45 minutes gm; at 195-200 page 17 / 29 pages 1013064654-0 100134551^ single number A〇101 201221521 ! 丨 °C mixing 2

I ____I hours. TMP: referred to herein as trimethyl phosphite. US Pat. No. 3,636,145 discloses mass production in high yield, high purity and very fast reaction rate and by transesterification involving tridecyl phosphite and alkanol. A method of preparing a trialkyl phosphite by a suitable method. The reaction is substantially carried out in the presence of a basic catalyst and in the presence of a non-azeotropic solvent. Surprisingly, the inventors of the present invention have found that the yield of the final product decreases in the catalyst and/or solvent. No. TMP (gm) Isodecyl alcohol (gm) Sodium methoxide (gm) -___ - Reaction conditions Yield (°/〇) ------ 1 63 316 0.45 Add TMP at 70-80 °C; Stir at -200 °C for 2 hours. 85.25 I i _____--— 2 63 316 Add TMP at 70-80 °C; stir at 195-200 °C for 2 hours. 93.82 3 63 316 0.45 Add at 70-80 °C _ __一 - 82.47 _____一 —------------ 10013455 Order No. A〇m Page 18 of 29 1013064654 -0 201221521

~~1 - TMP; stirred at 85-90 ° C for 9 hours; stirred at 195-200 ° C for 2 hours. 4 63 316 —— — at 70-80. (: Add TMP; stir at 85-90 ° C for 9 hours; stir at 195-200 ° C for 2 hours. 94 Obtain evidence from Table 2 that 'when the reaction is carried out in the absence of an inert catalyst', the product is obtained. Higher yield. Even in the absence of the non-co-solvent, the yield of the reaction is higher. I. 丨 4-14 The following table shows the molecular formula IU sterol with carbon chain enthalpy and the use of the trioxane of formula II. The experiment conducted by the phosphite, the alkyl alcohol of the formula III and the trialkyl phosphite of the formula 11 are selected from the group consisting of 100134551^^^^〇 101 page 19/29 pages 1013064654-0 201221521 -c3 carbon atoms a base moiety. The dialkyl phosphite is added to the alkanol at about 75 ϊ(:_ιι(Γ{^ elevated temperature, and then the reaction temperature is raised to about 195X-2HTC, and at the same temperature Stir for about 2-4 hours to give the desired trialkyl phosphite. The respective trialkyl linoleate was obtained in more than 850/〇 yield. Observed when using a higher grade like Cm In the case of alcohols, the reaction does not proceed at the desired rate and the desired yield. M The amount of raw material used is CTMP/TEP /TIPP) Force α into temperature C TMP/T EP/TIPP ) Stage 1 TIVIP/TE P/TIPP Addition time (stage 1) Pity temperature stage 2 Recovery of alkaloids Final Product Ά % yield 102 gm 217 gm 86.45 4 TMP = 62 gm Isodecyl alcohol - 316 gm were mixed at room temperature for 〇 min - at 19 〇 z 〇〇 ° c 卞 2 hours - 5 99 gm 182 gm 86.95 TMP = 62 gm xin Yeast ^eigm 95-1050C 4 hours 15 minutes shovel at 18U 2 hours 77 gm 192 gm 91.72 6 , TMP-e2gm octanol = 261gm 98-101 4 hours 2 〇 3 &quot; C 2 hours ___ — Polymerization TMP=s31gm Eighteen yeast=271 gm 95-100°C 3 hours 40 minutes Z6〇〇C 卞3 hours—polymerization Λ 8 TMP=23gm octadecyl alcohol s=200gm 95-1000C 3 hours 30 minutes nickel-\&amp ;Cb 22&^C 2 hours 63 gm 104 gm 87.33 9 TMP=22gm 1-fourteen yeast=161gm 95-1030C 3 hours 2〇2&quot;C 2 hours l〇〇m55 order number A0101 Page 20/ Total 29 tribute 1013064654-0 201221521 [0006] Ο [0007]

10 TMP=22gm 1-tetradecyl alcohol = 161gm 94-101 °C 4 hours at 190-200 ° C for 2 hours 62 gm 103 gm 87.49 11 TMP-21gm [ cetyl alcohol = 168 gm 95-100^0 3 Hour at 190-2O0 °C for 2 hours 58 gm 114 gm 89.12 12 TMP = 21 gm Ί-cetyl alcohol = 168 gm 95-1000 C 4 hours at 190-202. . 2 hours 57 gm 115 gm 90.08 13 TEP=84gm isodecyl alcohol = 316gm 95-1000C 4 hours 30 minutes at 190-202eC 2 hours 92 gm 240 gm 95.61 14 TIPP=84gm isodecyl alcohol = 250gm 95-1 QO° C 4 hours 15 minutes at 191-2000C 2 hours 92 gm 170 gm 89.26 ΤΜΡ: referred to herein as tridecyl phosphite ΤΕΡ: referred to herein as triethyl phosphite ΤΙΡΡ: as referred to herein Is the triisopropyl phosphite phenol content All of the samples prepared above were analyzed for their purity. 041变化。 The acid value (mgKOH / gm) was changed at 0. 0072-0. The weight of the sample changed from 0. 8866 to 0. 8905. Surprisingly, the phenol content found in all of the prepared samples was NIL. The foregoing references are directed to compositions having known equivalents, and such equivalents are incorporated herein by reference. Therefore, it will be apparent that changes may be made to the above described aspects and embodiments of the invention without departing from the principles of the teachings herein. The additional advantages of the present invention will become apparent to those skilled in the art after considering the principles of the particular form discussed and illustrated. Therefore, it is understood that the invention is not limited to the specific embodiment shown or described, but is intended to be a substitute or modification within the scope of the invention. 1(){) 134551^Single number A0101 Page 21 of 29201221521 [Simplified illustration] [0008] [Explanation of main component symbols] [0009] 100134551^^ A〇101 Page 22 of 29 1013064654 -0

Claims (1)

201221521 VII. Patent Application Range: 1. An improved method for preparing a trialkyl phosphite of formula I: 1-R 〇0-3⁄4 IP - 1 \o R The method comprises a trialkyl group of formula 11 The phosphite R ο / \o - RP \o R is reacted with the alkanol f-OH of the formula III such that R1 represents an alkyl moiety having 8 to 16 carbon atoms, and R represents 1 to 3 a monoalkyl moiety of one carbon atom. 2. The method of claim 1, wherein the trialkyl phosphite of formula 11 is reacted with the alkanol rLoh in the absence of a catalyst or lack of a solvent or lack of a catalyst and a solvent. 3. The method of claim 1, wherein the trialkyl phosphite of the formula II is added to the damolol at a temperature ranging from 75 °C to 180 °C. 4. The method of claim 3, wherein the alkyl phosphite is added to the molecular formula of the alkanol 10013455 during a period of 0.5-7 hours! The method of claim 1, wherein the alkyl sulfonate and the alkanol are in a molar ratio of 1:3 to 1:5. Added. 6. The method of claim 2, wherein the alcoholic alcohol of the formula is selected from the group consisting of isodecyl alcohol, isotrienol, octanol, tetradecanol, and cetyl alcohol. 7. The method of claim 1, wherein the trialkyl phosphite of formula II is selected from the group consisting of triethyl phosphite, trimethyl phosphite, and triisopropyl sulphate. . 8. The method of claim 1, further comprising the step of recovering the alcohol by-product R-0H of the formula IV by condensation. 9. An improved process for the preparation of a trialkyl phosphite of formula I: Rv 〇 \ \ 1 R1 The method comprises: (a) by formulating a temperature at a temperature between 77.000.8 The compound of hydrazine is added to the alkanol ri_〇h, and the trialkyl phosphite of formula II R\0-R 0-P \ 〇IR 1013064654-0 1〇0丨3455 is produced as a single bat number A0101 1丨24 pages/total 29 pages 201221521 The calcined alcohol rl〇h of the knife formula 1u is reacted such that R1 represents a monoalkyl moiety having 8 to 16 carbon atoms, and R represents a one having 1 to 3 carbon atoms. An alkyl moiety; (6) the reaction material is maintained at a temperature above at least one of the ani alcohols having from i to 3 carbon atoms for a predetermined period of time while the reaction is removed synchronously An alcohol by-product, DiH; and (c) the target compound by a molecular recovery formula. 10. For example, please refer to the financial method described in Item 9 of the patent, in which the formula is in the absence of a catalyst or lack of a solvent or a catalyst and a solvent. The method of claim 9, wherein the temperature above the boiling point of the alcohol by-product is from 18 〇χ. To about 220 baht. 12. The method of claim 9, wherein the predetermined time period is from about 2 hours to about 4 hours. 13. The method of claim 9, comprising cooling the reaction material obtained at the end of step (a) in an inert gas before subjecting it to step (b). 14. An improved process for the preparation of a trialkyl phosphite of formula I: &lt; 0-R1 0 - P: 〇100134551^ singly numbered 1 Page 25 of 29 1013064654-0 201221521 The method comprises : (a) by at 75. 〇180. At a temperature between 〇, a compound of the formula 缓慢 is slowly added to the allylic alcohol RLOH at a temperature of at least 0.5 mM, and the compound of the formula 丨丨 is added to the phenol Thereafter, the trialkyl phosphite of formula II 〇-p οIR is reacted with an alkanol R1-0H of formula III such that R1 represents an alkyl moiety having 8 to 16 carbon atoms, and R represents an alkyl moiety having 1 to 3 carbon atoms (b) simultaneously maintaining the reaction mass for at least a temperature above the boiling point of the monoalkanol having 1 to 3 carbon atoms for a predetermined period of time to synchronously remove the alcohol pair produced during the reaction Product R—〇H; (c) optionally cooling the reaction product under an inert gas; (d) heating the cooled reaction product to 190-2 G00C under a vacuum of 2 mm for a sufficient period of time; And (e) cooling the reaction product to a temperature of about 400 C and recovering the compound of formula I by filtration. 15. The method of claim 14, wherein the trialkyl phosphite having a molecular formula of π is in a period of from about 0.5 hours to about 6 hours. 10013455^^^^ A〇101 Page 26/ A total of 29 pages 1013064654-0 201221521, is added to the alkanol of the formula 大约 at a temperature of about 75 ° C-18. 16 . 17 · 18 . (\ 19 . Ο 20 . 21 . 22 The method of claim 14, wherein the trimethyl phosphite of the formula is reacted with the alkanol in the absence of a catalyst or lack of a solvent or a catalyst and a solvent. The method of claim 14 wherein the temperature above the boiling point of the alkanol having one of 1 to 3 carbon atoms is from about 195 C to 210 ° C. As described in claim 14 The method wherein the reaction mass is maintained at the temperature for from about 2 to about 4 hours. A trialkyl phosphite of formula I: It allows R 1 to represent a monoalkyl moiety having 8 to 16 carbon atoms, wherein the compound of formula I is substantially free of a phenolic impurity. The trialkyl phosphite of the formula I according to claim 18, wherein the compound of the formula I is completely free of a phenolic impurity. The trialkyl phosphite of the formula 1 according to claim 19, wherein the compound of the formula I contains less than 100 ppm of a phenolic impurity. An improved process for the preparation of trialkyl phosphites of formula I. 10013455^.Single number A0101 Page 27/29 guest 1013064654-0 201221521 The trialkyl phosphite of formula i is substantially as herein described The example describes: °-Px 〇 1001345#单单 A〇101 Page 28 of 29 1013064654-0