Реакция #570288

Уравнение реакции

hydrochloric acid

ethyl chloroformate

thiomorpholin-3-one

lithium diisopropylamide

→

3-oxothiomorpholine-2-carboxylic acid ethyl ester

Выход 80.0%

Растворители

tetrahydrofuran

Условия реакции

Обработка

1. 1
   workup.STIRRINGAfter 1 to 3 hours' stirring
2. 2
   Концентрированиеconcentrated
3. 3
   workup.ADDITIONdiluted with ethyl acetate
4. 4
   Промывкаwashed with water
5. 5
   Другоеdried
6. 6
   Концентрированиеconcentrated

Методика

A mixture of thiomorpholin-3-one (1 equivalent), tetrahydrofuran (5-40 parts), and lithium diisopropylamide (1-2 equivalents) is stirred at -10° to 50° C. for 1 to 3 hours. To this mixture is added ethyl chloroformate (1 to 2 equivalents). After 1 to 3 hours' stirring, the mixture is acidified with hydrochloric acid, concentrated, diluted with ethyl acetate, washed with water, dried, and concentrated to give 3-oxothiomorpholine-2-carboxylic acid ethyl ester in 80 to 90% yield.

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