HRID628462

反应详情

EQUATION

反应方程式

HRID 628462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-(4-fluorophenyl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole (44.5 g, 0.22 mol) in 600 mL chloroform is added at 0° C. N-bromosuccinimide (117 g, 0.66 mol). The mixture is stirred 17 h at RT. Thereafter, the mixture is diluted with water and extracted with dichloromethane. The combined organic phases are dried and evaporated. The obtained crude material is purified by column chromatography on silica (6 cm×40 cm, eluent dichloromethane). The obtained product is further purified by trituration with a MTBE-hexane mixture and 38.2 g (61%) of the product are obtained as solid.

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. customThe combined organic phases are dried
  3. customevaporated
  4. customThe obtained crude material
  5. customis purified by column chromatography on silica (6 cm×40 cm, eluent dichloromethane)
  6. customThe obtained product is further purified by trituration with a MTBE-hexane mixture and 38.2 g (61%) of the product
  7. customare obtained as solid