HRID2237455

反应详情

EQUATION

反应方程式

HRID 2237455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of the product from step c.) (6.4 g, 35 mmol) in dry THF (400 ml) was cooled to 0° C. and a 1.0 M solution of BH3 in THF (174 ml, 174 mmol) was added dropwise over 10 minutes. After the addition was complete the mixture was stirred for an additional 20 minutes at 0° C. and then warmed to 22° C. for 2 hours. Next, the mixture was poured into ice cold sat. NaHCO3 (300 ml) and extracted with EtOAc (2×200 ml). The organic layer was dried (MgSO4) and concentrated providing 3.58 g (65%) of the subtitle compound. MS: ESI (positive): 157 (M+H).

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturewarmed to 22° C. for 2 hours
  3. extractionextracted with EtOAc (2×200 ml)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. concentrationconcentrated