SU311922A1 - METHOD FOR OBTAINING PHOSPHORYLATED ACYLALES ' - Google Patents
METHOD FOR OBTAINING PHOSPHORYLATED ACYLALES 'Info
- Publication number
- SU311922A1 SU311922A1 SU1422242A SU1422242A SU311922A1 SU 311922 A1 SU311922 A1 SU 311922A1 SU 1422242 A SU1422242 A SU 1422242A SU 1422242 A SU1422242 A SU 1422242A SU 311922 A1 SU311922 A1 SU 311922A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- acylales
- phosphorylated
- obtaining
- obtaining phosphorylated
- acylals
- Prior art date
Links
- 150000008063 acylals Chemical class 0.000 description 4
- DTQVDTLACAAQTR-UHFFFAOYSA-N trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing Effects 0.000 description 2
- -1 (phosphinyl) ethyl Chemical group 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000001188 haloalkyl group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- ILZUMOMDNFYVSY-UHFFFAOYSA-N methoxy(phenyl)phosphane Chemical compound COPC1=CC=CC=C1 ILZUMOMDNFYVSY-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Изобретение относитс к способу получени фосфорилированных ацилалей, которые представл ют интерес дл изучени их физиологической активности.The invention relates to a process for the preparation of phosphorylated acylals, which are of interest for studying their physiological activity.
Предлагаемый способ получени фосфорилированных ацилалей общей формулыThe proposed method for producing phosphorylated acylals of the general formula
PCH,CH,OCH-OCR,PCH, CH, OCH-OCR,
R/ IIIIIR / IIIII
ОСН, оOch o
где R, RI - алкил, арил, алкоксил,where R, RI is alkyl, aryl, alkoxy,
Ra - алкил, галоидалкил, основан на взаимодействии винил-р-(фосфинил )-этиловых эфировRa - alkyl, haloalkyl, based on the interaction of vinyl-p- (phosphinyl) -ethyl esters
КTO
PCHsCH,OCH CH,PCHsCH, OCH CH,
R.R.
с карбоновыми кислотами (лучшие результаты получены с трифторуксусной кислотой).with carboxylic acids (best results are obtained with trifluoroacetic acid).
Синтез ацилалей, не содержащих фосфора, описан, однако метод получени фосфорилированных ацилалей из вииил-р-(фосфинил)этиловых эфиров так же, как и сами соединени , вл етс новым.The synthesis of phosphorus-free acylals has been described; however, the method for producing phosphorylated acylals from viyl-p- (phosphinyl) ethyl esters, as well as the compounds themselves, is new.
Синтез провод т в четырехгорлой колбе, снабженной мешалкой, обратным холодильником , капельной воронкой и термометром, опущенным до дна колбы. В колбу помешают 2,08 г (0,01 моль), из капельной воронки добавл ют 1,14 г (0,1 люль) трифторуксусной кислоты. Температура смеси повышаетс с 20 до 34°С. Реакционную смесь перемешивают до снижени температуры до исходной. При разгонке в вакууме собирают 1,7 г целевого продукта (52,8% от теории), т. кип. 110°С при 0,7 мм рт. ст., 1,4485; df 1,30; MR: найдено 66,88, вычислено 66,43.The synthesis is carried out in a four-necked flask equipped with a stirrer, a reflux condenser, an addition funnel and a thermometer dipped to the bottom of the flask. 2.08 g (0.01 mol) is stirred into the flask, and 1.14 g (0.1 ly) of trifluoroacetic acid is added from the dropping funnel. The temperature of the mixture rises from 20 to 34 ° C. The reaction mixture is stirred to reduce the temperature to the original. During distillation in vacuum, 1.7 g of the desired product are collected (52.8% of theory), i.e. bale. 110 ° C at 0.7 mm Hg. Art., 1,4485; df 1.30; MR: found 66.88, calculated 66.43.
Найдено, %: Р 9,80, 10,04.Found,%: P 9.80, 10.04.
Вычислено, О : Р 9,63.Calculated O: P 9.63.
Пример 2. Получение р-(метоксифенилфосфинил ) -этоксиэтилндентрифторацетата (4метил-8-фенил-1 ,1,1-трифтор - 3,5,9-триокса - 8 фосфадекандиоиа-2 ,8)Example 2. Obtaining p- (methoxyphenylphosphine) -ethoxyethyltinfluoroacetate (4methyl-8-phenyl-1, 1,1-trifluoro-3,5,9-triox-8 phosphadecanedio-2, 8)
сн,о.noo, oh.
)рсн,сн,-о) RSN, SN, -O
С,Н, II)СН-СН,C, H, II) CH-CH,
о РзССОAbout RZSSO
Реакцию привод т в услови х примера 1. 3 гревают 3 час на вод ной бане, нагретой до 60°С, при посто нном неремешивании. При. нерегонке выдел ют 1,4 г (41,2% от теории) целевого продукта. Т. кин. 188°С при: 0,5 мм рт. ст., ng 1,4967, d4°l,32; MR: найдено5 75 13 вычислено 7498. Пайдено, %: Р 9,43, 9,30. Вычислено, %: Р 9,12. . 4 , Предмет изобретени 1. Снособ получени фосфорилированных ацидалей, отличающийс тем, что винил-р (фосфинил)-этиловый эфир подвергают взаимодействию с карбоновой кислотой. 2. Способ по п. 1, отличающийс тем, что нроцесс ведут при нагревании до 60°С.The reaction is carried out under the conditions of Example 1. 3 are heated for 3 hours in a water bath heated to 60 ° C, with constant unmixing. At. non-distillation, 1.4 g (41.2% of theory) of the desired product are recovered. T. Kin. 188 ° C at: 0.5 mm Hg. Art., ng 1.4967, d4 ° l, 32; MR: found 75 75 13 calculated 7498. Paideno,%: P 9.43, 9.30. Calculated,%: P 9,12. . 4, the subject matter of the invention 1. A process for the preparation of phosphorylated acidals, characterized in that the vinyl-p (phosphinyl) ethyl ester is reacted with a carboxylic acid. 2. A method according to claim 1, characterized in that the process is carried out by heating to 60 ° C.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU311922A1 true SU311922A1 (en) |
Family
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