2-bromine-2, 2-difluoroacetic acid acetonylidene protected monoglyceride, waterborne polyurethane and preparation method thereof
A technology of acetone acetone and difluoroacetate is applied in the field of printing and dyeing auxiliaries, which can solve the problems of yellowing of textiles, easy water absorption and moisture regain, poor flame retardancy and the like
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[0029] The present invention provides a method for preparing 2-bromo-2,2-difluoroacetone acetone-protected monoglyceride according to the above scheme, comprising the following steps: condensing 2-bromo-2,2-difluoroacetate, acetone Glycerol and basic catalyst are mixed to carry out transesterification reaction to obtain 2-bromo-2,2-difluoroacetone acetone mono-protected monoglyceride having the structure described in formula I;
[0030] The molar ratio of the 2-bromo-2,2-difluoroacetate to acetone acetal is 1:1-5.
[0031] In the present invention, without special instructions, the raw materials used are all commercially available commodities well known in the art.
[0032] In the present invention, the 2-bromo-2,2-difluoroacetate is preferably methyl 2-bromo-2,2-difluoroacetate or ethyl 2-bromo-2,2-difluoroacetate. The basic catalyst preferably includes one or more of hydroxide, carbonate, bicarbonate, sodium hydride and sodium alkoxide, more preferably includes alkali metal...
Embodiment 1
[0070] In a 1L reaction vessel equipped with a thermometer, reflux condenser, water separator and stirrer, add 203 g of ethyl 2-bromo-2,2-difluoroacetate, 260 g of acetone acetal, 3.2 g of sodium methoxide, and at 115 g The reaction was carried out for 12 hours at ℃, and the obtained reaction product was subjected to vacuum distillation to collect fractions under the conditions of 104-106 ℃ / 25 mmHg to obtain 2-bromo-2,2-difluoroacetone acetone monoprotected glycerol having the structure shown in formula I. The ester was 285.5 g, the yield was 98.8%, and the purity was 99.5%.
[0071]
[0072] The 2-bromo-2,2-difluoroacetone triglyceride prepared in Example 1 was subjected to nuclear magnetic analysis, and the results were as follows Figure 1 ~ Figure 2 shown, where figure 1 is the NMR spectrum, figure 2 for the nuclear magnetic fluoride spectrum. Depend on Figure 1 ~ Figure 2 It can be seen that the 2-bromo-2,2-difluoroacetone acetonide-protected monoglyceride prepar...
Embodiment 2
[0077] 189 g of methyl 2-bromo-2,2-difluoroacetate, 260 g of acetone acetal, 1.89 g of potassium hydroxide were added to a 1 L reaction vessel equipped with a thermometer, reflux condenser, water separator and agitator. The reaction was carried out at 125° C. for 8 hours, and then the obtained reaction product was subjected to vacuum distillation to collect fractions under the condition of 104-106° C. / 25 mmHg to obtain 283.3 g of 2-bromo-2,2-difluoroacetone acetone-protected monoglyceride. The yield is 98.0% and the purity is 99.5%.
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