CN104045566A - Fatty acid ester compounds of 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol and synthesis method thereof - Google Patents
Fatty acid ester compounds of 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol and synthesis method thereof Download PDFInfo
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Abstract
The invention relates to fatty acid ester compounds of 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol and a synthesis method thereof. According to the method, with DCC (dicyclohexylcarbodiimide) as a dehydrating agent and DMAP (dimethylaminopyridine) as an activating agent, 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol is adopted as the raw material to synthesize 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol tetralaurate, 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol hexatetracontanic ester, 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol tetrastearate, and 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol(12-hydroxystearic acid)ester with lauric acid, hexadecanoic acid, stearic acid and 12-hydroxystearic acid respectively at room temperature. <1>HNMR and IR are employed to characterized structures of the target products. Dichloromethane and DMF solvents are employed to undergo esterification reaction respectively, and the mole ratio of 2, 3-dihydroxymethyl- 2, 3-dinitro-1, 4-butanediol to fatty acid is 1:4-6, the mole ratio of DCC to 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol is 3-5:1, and the mole ratio of DMAP to 2, 3-dihydroxymethyl-2, 3-dinitro-1, 4-butanediol is 0.05-0.2:1.
Description
Technical field
The present invention relates to 2,3-dihydroxymethyl-2,3-dinitrobenzene-1, the fatty acid ester compound of 4-butyleneglycol and synthetic method thereof, particularly 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four laurates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four Palmitates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO tetrastearate, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four (12-oxystearic acid) ester and synthetic, belongs to organic chemistry filed.
Background technology
Polyhydric alcohol fatty acid ester has good thermotolerance and oilness, and it can be both as the plastic plasticizer under high temperature process and working conditions, also can be used as basic ester for the synthesis of lubricated class oil product.The polyhydric alcohol fatty acid ester that contains hydroxyl is a kind of well emulsifying agent, has sizable practical value.
Four kinds of compounds 2 of synthesized of the present invention, 3-dihydroxymethyl-2, 3-dinitrobenzene-1, 4-butyleneglycol four laurates, 2, 3-dihydroxymethyl-2, 3-dinitrobenzene-1, 4-butyleneglycol four Palmitates, 2, 3-dihydroxymethyl-2, 3-dinitrobenzene-1, 4-butyleneglycol tetrastearate, 2, 3-dihydroxymethyl-2, 3-dinitrobenzene-1, 4-butyleneglycol four (12-oxystearic acid) ester, all belong to polyhydric alcohol fatty acid ester, and 2, 3-dihydroxymethyl-2, 3-dinitrobenzene-1, 4-butyleneglycol four (12-hydroxy stearic acid ester) is the polyhydric alcohol fatty acid ester that contains four hydroxyls, be expected to become a kind of novel emulsifying agent, and in molecular structure, contain two nitros, can there is certain contribution to the energy of emulsion explosive system.
The current synthetic report that has no about these four kinds of fatty acid esters.And similar compound synthetic generally to adopt polyvalent alcohol and lipid acid be raw material, the vitriol oil, tosic acid or solid super-strong acid are that catalyzer reacts, abroad report recently taking methylene dichloride as solvent, dicyclohexylcarbodiimide (DCC) is dewatering agent, DMAP (DMAP) is catalyzer, the synthetic tetrahydroxybutane fatty acid ester of at room temperature reaction and pentaerythritol fatty ester.
Summary of the invention
The object of the present invention is to provide a kind of 2,3-dihydroxymethyl-2, the fatty acid ester compound of 3-dinitrobenzene-BDO and synthetic method thereof.
The technical scheme that realizes the object of the invention is: a kind of 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol fat acid esters compound, described fat acid esters compound is 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four laurates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four Palmitates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO tetrastearate, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four (12-oxystearic acid) ester, its chemical structural formula is as follows respectively:
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four laurates
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four Palmitates
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO tetrastearate
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four (12-oxystearic acid) ester
The one 2 of said structure, 3-dihydroxymethyl-2, the synthetic route of 3-dinitrobenzene-BDO fatty acid ester compound is as follows:
Wherein R is for being respectively C
12h
23, C
16h
31, C
18h
35, C
18h
35o.
A kind of 2,3-dihydroxymethyl-2,3-dinitrobenzene-1, the fatty acid ester compound of 4-butyleneglycol is prepared by the following method: under room temperature, by 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol and lipid acid are placed in organic solvent, and its mol ratio is 1:4～6, add dewatering agent DCC and catalyzer DMAP reaction.
Described lipid acid is lauric acid, palmitic acid, stearic acid or 12-oxystearic acid.
The organic solvent of described esterification adopts methylene dichloride or DMF, described dewatering agent and 2,3-dihydroxymethyl-2, the mol ratio of 3-dinitrobenzene-BDO is 3 ~ 5:1, described catalyzer and 2,3-dihydroxymethyl-2, the mol ratio of 3-dinitrobenzene-BDO is 0.05 ~ 0.2:1.
Compared with prior art, the present invention has the following advantages:
1. 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four laurates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four Palmitates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO tetrastearate, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four (12-oxystearic acid) ester there is not yet bibliographical information.
2. in the molecule of four kinds of esters, all contain two nitros, and symmetrical configuration, molecular stability is good, and 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four (12-oxystearic acid) ester is the polyhydric alcohol fatty acid ester that contains four hydroxyls, can be used as a kind of novel emulsifying agent and uses.
3. avoid the use of an acidic catalyst, saved the operation such as alkali cleaning, washing, reduced the generation of a large amount of waste water, reduced the pollution to environment.Therefore, there is certain economy and the feature of environmental protection.
4. reaction is at room temperature carried out, and has avoided the generation of the side reaction such as oxidation under high temperature.Therefore, saved the harsh reaction conditions of nitrogen protection, reaction is reduced equipment requirements.
5. thick product, by recrystallizing and refining, is conducive to suitability for industrialized production.
Brief description of the drawings
Fig. 1 is embodiment 12,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four laurates
1h NMR.
Fig. 2 is embodiment 12,3-dihydroxymethyl-2, the IR of 3-dinitrobenzene-BDO four laurates.
Fig. 3 is embodiment 52,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four Palmitates
1h NMR.
Fig. 4 is embodiment 52,3-dihydroxymethyl-2, the IR of 3-dinitrobenzene-BDO four Palmitates.
Fig. 5 is embodiment 92,3-dihydroxymethyl-2,3-dinitrobenzene-BDO tetrastearate
1h NMR.
Fig. 6 is embodiment 92,3-dihydroxymethyl-2, the IR of 3-dinitrobenzene-BDO tetrastearate.
Fig. 7 is embodiment 13 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four (12-oxystearic acid) ester
1h NMR.
Fig. 8 is embodiment 13 2,3-dihydroxymethyl-2, the IR of 3-dinitrobenzene-BDO four (12-oxystearic acid) ester.
Embodiment
Embodiment 1
2,3-dihydroxymethyl-2, the preparation of 3-dinitrobenzene-BDO four laurates
2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol (its preparation method is shown in Wang Juan, Liu great Bin, Zhou Xinli. 1,4-bis-nitrine-2,3-bis-azido-methyl-2, synthetic [J] of 3-dinitrobutane. explosive, 2012,41 (4): 1-4.) (1mmol, 0.24g), lauric acid (6mmol, 1.2g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 78.8%.
Fig. 1 from brief description of the drawings and Fig. 2 can find out,
1h NMR (400 MHz, CDCl
3) δ 4.85,4.81,4.78,4.74 (dd,
j=12.4,
j=12.4,8H), 2.25,2.27,2.29 (t,
j=7.6,8H), 1.57,1.55,1.53 (t,
j=8.4,8H), 1.29,1.25 (d,
j=17.2,64H), 0.86,0.88,0.89 (t,
j=7.2,12H). IR 2916 (s, CH
2), 2848 (s, CH
2), 1749 (s, C=O), 1566 (s, NO
2), 1461 (s, CH
3), 1392 (s, CH
3), 1149 (s, C – O), 720 (s).
Embodiment 2
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), lauric acid (4mmol, 0.8g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 67.1%.
Embodiment 3
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), lauric acid (6mmol, 1.2g), DMF 10mL, DCC(3mmol, 0.618g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 54.9%.
Embodiment 4
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), lauric acid (6mmol, 1.2g), DMF 10mL, DCC(5mmol, 1.03g), DMAP(0.05mmol, 0.0061g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 64.4%.
Embodiment 5
2,3-dihydroxymethyl-2, the preparation of 3-dinitrobenzene-BDO four Palmitates
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), palmitic acid (6mmol, 1.536g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 79.6%.
Fig. 3 from brief description of the drawings and Fig. 4 can find out,
1h NMR (500 MHz, CDCl
3) δ 4.85,4.83 (d,
j=12.4,4H), 4.79,4.76 (d,
j=12.35,4H), 2.27,2.28,2.30 (t,
j=7.55,8H), 1.57,1.55 (d,
j=9.3,8H), 1.31 (s, 96H), 0.87,0.89,0.90 (t,
j=7.05,12H). IR 2916 (s, CH
2), 2848 (s, CH
2), 1750 (s, C=O), 1566 (s, NO
2), 1462 (s, CH
3), 1392 (s, CH
3), 1149 (s, C – O), 719 (s).
Embodiment 6
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), palmitic acid (4mmol, 1.024g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 67.7%.
Embodiment 7
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), palmitic acid (6mmol, 1.536g), DMF 10mL, DCC(3mmol, 0.618g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 55.1%.
Embodiment 8
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), palmitic acid (6mmol, 1.536g), DMF 10mL, DCC(5mmol, 1.03g), DMAP(0.05mmol, 0.0061g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 66.6%.
Embodiment 9
2,3-dihydroxymethyl-2, the preparation of 3-dinitrobenzene-BDO tetrastearate
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), stearic acid (6mmol, 1.704g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 81.4%.
Fig. 5 from brief description of the drawings and Fig. 6 can find out,
1h NMR (500 MHz, CDCl
3) δ 4.76,4.79,4.83,4.85 (dd,
j=12.4,
j=12.4,8H), 2.27,2.28,2.30 (t,
j=7.55,8H), 1.56 (s, 8H), 1.26,1.31 (d,
j=22.8,112H), 0.87,0.89,0.90 (t,
j=7.1,12H). IR 2917 (s, CH
2), 2848 (s, CH
2), 1750 (s, C=O), 1567 (s, NO
2), 1463 (s, CH
3), 1393 (s, CH
3), 1176 (s, C – O), 719 (s).
Embodiment 10
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), stearic acid (4mmol, 1.136g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 69.9%.
Embodiment 11
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), stearic acid (6mmol, 1.704g), DMF 10mL, DCC(3mmol, 0.618g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 58.9%.
Embodiment 12
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), stearic acid (6mmol, 1.704g), DMF 10mL, DCC(5mmol, 1.03g), DMAP(0.05mmol, 0.0061g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 70.1%.
Embodiment 13
2,3-dihydroxymethyl-2, the preparation of 3-dinitrobenzene-BDO four (12-oxystearic acid) ester
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), 12-oxystearic acid (6mmol, 1.8g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 79.9%.
Fig. 7 from brief description of the drawings and Fig. 8 can find out,
1h NMR (400 MHz, CDCl
3) δ 4.74,4.78,4.81,4.85 (dd,
j=12.4,
j=12.4,8H), 3.58 (s, 4H), 2.25,2.27,2.29 (t,
j=7.6,8H), 1.48,1.46,1.42,1.38 (dd,
j=8,
j=16.8,28H), 1.26 (s, 88H), 0.86,0.88,0.89 (t,
j=7.2,12H). IR 3324 (m, OH), 2917 (s, CH
2), 2848 (s, CH
2), 1750 (s, C=O), 1569 (s, NO
2), 1467 (s, CH
3), 1393 (s, CH
3), 1179 (s, C – O), 720 (s).
Embodiment 14
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), 12-oxystearic acid (4mmol, 1.2g), methylene dichloride 10mL, DCC(5mmol, 1.03g), DMAP(0.2mmol, 0.024g), 2,3 stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 68.1%.
Embodiment 15
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), 12-oxystearic acid (6mmol, 1.8g), DMF 10mL, DCC(3mmol, 0.618g), DMAP(0.2mmol, 0.024g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 55.9%.
Embodiment 16
2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO (1mmol, 0.24g), 12-oxystearic acid (6mmol, 1.8g), DMF 10mL, DCC(5mmol, 1.03g), DMAP(0.05mmol, 0.0061g), stirring at room temperature, TLC follows the tracks of, and treats 2,3-dihydroxymethyl-2, when 3-dinitrobenzene-BDO reacts completely, stopped reaction.100mL (2 × 50mL) CHCl
3product is extracted, collect CHCl
3phase, concentrating under reduced pressure, crude product is through recrystallizing methanol, then uses acetone recrystallization.Yield is 67.2%.
Claims (9)
1. one kind 2,3-dihydroxymethyl-2,3-dinitrobenzene-1, the fatty acid ester compound of 4-butyleneglycol, is characterized in that described compound is 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four laurates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-1,4-butyleneglycol four Palmitates, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO tetrastearate, 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO four (12-oxystearic acid) ester, its chemical structural formula is as follows respectively:
、
、
、
。
2. according to claim 12,3-dihydroxymethyl-2, the fatty acid ester compound of 3-dinitrobenzene-BDO, is characterized in that described compound prepared by following methods: under room temperature, by 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO and lipid acid are placed in organic solvent, its mol ratio is 1:4～6, adds dewatering agent DCC and catalyzer DMAP reaction.
3. according to claim 22,3-dihydroxymethyl-2,3-dinitrobenzene-BDO fatty acid ester compound, is characterized in that in described esterification, organic solvent adopts methylene dichloride or DMF.
4. according to claim 22,3-dihydroxymethyl-2,3-dinitrobenzene-BDO fatty acid ester compound, is characterized in that described dewatering agent and 2,3-dihydroxymethyl-2, the mol ratio of 3-dinitrobenzene-BDO is 3 ~ 5:1.
5. according to claim 22,3-dihydroxymethyl-2,3-dinitrobenzene-BDO fatty acid ester compound, is characterized in that described catalyzer and 2,3-dihydroxymethyl-2, the mol ratio of 3-dinitrobenzene-BDO is 0.05 ~ 0.2:1.
6. one kind 2,3-dihydroxymethyl-2, the synthetic method of 3-dinitrobenzene-BDO fatty acid ester compound, is characterized in that said method comprising the steps of: under room temperature, by 2,3-dihydroxymethyl-2,3-dinitrobenzene-BDO and lipid acid are placed in organic solvent, its mol ratio is 1:4～6, adds dewatering agent DCC and catalyzer DMAP reaction.
7. according to claim 62,3-dihydroxymethyl-2, the synthetic method of 3-dinitrobenzene-BDO fatty acid ester compound, is characterized in that in described esterification, organic solvent adopts methylene dichloride or DMF.
8. according to claim 62,3-dihydroxymethyl-2, the synthetic method of 3-dinitrobenzene-BDO fatty acid ester compound, is characterized in that described dewatering agent and 2,3-dihydroxymethyl-2, the mol ratio of 3-dinitrobenzene-BDO is 3 ~ 5:1.
9. according to claim 62,3-dihydroxymethyl-2,3-dinitrobenzene-1, the synthetic method of 4-butyleneglycol fat acid esters compound, is characterized in that described catalyzer and 2,3-dihydroxymethyl-2, the mol ratio of 3-dinitrobenzene-BDO is 0.05 ~ 0.2:1.
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| CN104496805A (en) * | 2015-01-09 | 2015-04-08 | 江苏大学 | Preparation method of octacosanol ester |
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| CN104496805A (en) * | 2015-01-09 | 2015-04-08 | 江苏大学 | Preparation method of octacosanol ester |
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