HRID456586

反应详情

EQUATION

反应方程式

HRID 456586 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of benzo[1,3]dioxol-5-yl-acetic acid (2.5 g, 13.9 mmol) in tetrahydrofuran (15 ml) under argon at −10° C. was treated dropwise with borane-dimethylsulfide complex (1.45 ml, 15.3 mmol). The mixture was stirred at ambient temperature for 1.5 hours (CAUTION—exothermic reaction). The orange solution was cooled to ˜5° C. (ice bath) and methanol (1.4 ml) was added. After 0.5 hour at room temperature, the mixture was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution. The organic extract was dried and evaporated to give a yellow oil (1.95 g, 84%).

WORKUP

后处理

  1. custom(CAUTION—exothermic reaction)
  2. additionwas added
  3. waitAfter 0.5 hour at room temperature
  4. customthe mixture was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution
  5. extractionThe organic extract
  6. customwas dried
  7. customevaporated