反应详情

温度

16.5 °C

461 g of sodium hydrogencarbonate and 350 g of (2S)-3-aminopropane-1,2-diol hydrochloride (VII) (commercially available) are initially charged at from 13 to 15° C. in 2.1 l of water and admixed with 950 ml of 2-methyltetrahydrofuran. 535.3 g of 5-chlorothiophene-2-carbonyl chloride (approx. 93%) in 180 ml of toluene are added dropwise to this mixture with cooling at from 15 to 18° C. over a period of two hours. For workup, the phases are separated and the organic phase is admixed in several steps with a total of 1.5 l of toluene. The precipitated product is filtered off with suction, washed with ethyl acetate and dried.

1. customFor workup, the phases are separated
2. filtrationThe precipitated product is filtered off with suction
3. washwashed with ethyl acetate
4. customdried