反应详情

温度

10 °C

In the following, tetrahydrofuran (THF) to be used was dehydrated on molecular sieves of 4 angstrom overnight. Inside of a 5 L four-neck flask was substituted with nitrogen gas and 2.2 kg of THF was placed therein, followed by cooling to 10° C. or lower. Then, 50 g of lithium aluminum hydride was placed therein and 250 g of ethyl 3,3-diethoxypropionate was added dropwise so that inner temperature did not exceed 10° C. After completion of the dropwise addition, temperature was elevated to 20° C. and reaction was carried out for 1 hour. After the reaction, 420 g of distilled water was added and the whole was stirred for 2 hours, then filtration was performed through No. 2 filtration paper, and subsequently a cake was washed with 1.1 kg of THF. The filtrate was concentrated at 40° C. to obtain 213 g of crude 3,3-diethoxy-1-propanol (hereinafter 33DEP).

1. customto be used was dehydrated on molecular sieves of 4 angstrom overnight
2. customdid not exceed 10° C
3. additionAfter completion of the dropwise addition, temperature
4. customwas elevated to 20° C.
5. customreaction
6. additionwas added
7. filtrationfiltration
8. filtration2 filtration paper
9. washsubsequently a cake was washed with 1.1 kg of THF
10. concentrationThe filtrate was concentrated at 40° C.