HRID1500147

反应详情

EQUATION

反应方程式

HRID 1500147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
155 °C

PROCEDURE

实验过程

In 1-(4-chlorobenzyl)-3,3-dimethyl-2-oxocyclopentane carboxylic acid methyl ester (1.5 g, 0.00509 mol), N,N-dimethylacetamide (1.5 mL) and pyridine hydrochloride (0.706 g, 0.00509×1.2 mol) were added and stirred at 155° C. for 4 hours. In the reaction liquid, pyridine hydrochloride (0.177 g, 0.00509×0.3 mol) was added and further stirred at 155° C. for another 6 hours. In the reaction liquid, toluene and saturated sodium bicarbonate water were added, and the mixture was partitioned. After extracting the aqueous layer using toluene, the organic layer was dried using anhydrous sodium sulfate and concentrated. Thereafter, the dried and concentrated product was purified using a silica gel column, and a target product was obtained.

WORKUP

后处理

  1. additionwas added
  2. stirringfurther stirred at 155° C. for another 6 hours
  3. additionwere added
  4. customthe mixture was partitioned
  5. extractionAfter extracting the aqueous layer
  6. customthe organic layer was dried
  7. concentrationconcentrated
  8. customThereafter, the dried
  9. customconcentrated product was purified
  10. customa target product was obtained