HRID1077591

反应详情

EQUATION

反应方程式

HRID 1077591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 17β-carbomethoxy-6-t-butylcarboxy-6-azaandrost-4-en-3-one (2.30 g, 5.33 mmol), Example 3, part E, in methylene chloride (70 mL) at -78° C. is treated with diisobutylaluminum hydride (1.5M in toluene, 15 mL, 22.5 mmol). After 20 minutes the reaction is quenched with methanol (4 mL), methylene chloride added (150 mL), washed with 2N NaOH and water, dried over MgSO4 and concentrated to give crude 17β-hydroxymethyl-3β-hydroxy-6-t-butylcarboxy-6-azaandrost-4-ene of sufficient purity to carry on to the following steps; yield: 2.16 g (99%).

WORKUP

后处理

  1. customAfter 20 minutes the reaction is quenched with methanol (4 mL), methylene chloride
  2. additionadded (150 mL)
  3. washwashed with 2N NaOH and water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated