HRID1363381

反应详情

EQUATION

反应方程式

HRID 1363381 的结构方程式

CONDITIONS

反应条件

温度
52.5 °C

PROCEDURE

实验过程

Compound of example 118 (15 g, 42 mmol) was subjected to hydroboration using NaBH4 (2.7 g, 71.4 mmol) and BF3-etherate (12.6 g, 88.8 mmol) in THF (50 mL). Excess diborane was destroyed by the addition of water. Conc. HCl (15 mL) was added and the reaction mixture was stirred at 50-55° C. for 1 h. It was cooled to room temperature The resulting mixture was made basic (pH 12-14) using an aqueous 50% NaOH solution. 30% H2O2 (9 mL) was added and the reaction mixture was stirred at 50-55° C. for 1 h. The reaction mixture was processed as described in example 2 to obtain the title compound.

WORKUP

后处理

  1. customExcess diborane was destroyed by the addition of water
  2. additionConc. HCl (15 mL) was added
  3. temperatureIt was cooled to room temperature The resulting mixture
  4. addition30% H2O2 (9 mL) was added
  5. stirringthe reaction mixture was stirred at 50-55° C. for 1 h