Реакция #55283

Уравнение реакции

3-carbethoxythiomorpholine

4-chloro-2-fluorophenylisocyanate

→

3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine

Выход 87.7%

Растворители

n-hexane

ether

Условия реакции

Обработка

1. 1
   ДругоеA heavy oil formed
2. 2
   workup.ADDITIONafter the addition
3. 3
   ДругоеThe oil crystallized
4. 4
   workup.STIRRINGafter stirring at room temperature for 15 min
5. 5
   ФильтрацияThe precipitate was collected by filtration

Методика

An emulsion of 14 g of 3-carbethoxythiomorpholine in 50 ml of n-hexane was added dropwise to a solution of 14 g of 4-chloro-2-fluorophenylisocyanate in 60 ml of anhydrous ether at 15° to 28° C. with stirring. A heavy oil formed after the addition. The oil crystallized after stirring at room temperature for 15 min. The precipitate was collected by filtration to give 24.3 g of 3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine, m.p. 111.5°-112.5° C.

Источник