HRID2285765

反应详情

EQUATION

反应方程式

HRID 2285765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The benzene solution of 1-isopropyl-3-azetidinylmethane sulfonate was added dropwise to the stirred refluxing toluene mixture containing the sodium salt of diphenylacetonitrile and refluxing continued for 1.5 hours after addition. The cooled reaction mixture was treated with water, the layers separated, and the organic layer extracted with dilute hydrochloric acid and water. The combined extracts were basified using dilute sodium hydroxide and the base insoluble material extracted with chloroform. The dried extract was concentrated and the residual material was recrystallized from isooctane. The α,α-diphenyl-α-(1-isopropyl-3-azetidinyl)acetonitrile weighed 142 g. (55%) and melted at 93°-95° C.

WORKUP

后处理

  1. temperaturerefluxing
  2. additionafter addition
  3. customThe cooled reaction mixture
  4. customthe layers separated
  5. extractionthe organic layer extracted with dilute hydrochloric acid and water
  6. extractionthe base insoluble material extracted with chloroform
  7. extractionThe dried extract
  8. concentrationwas concentrated
  9. customthe residual material was recrystallized from isooctane