HRID2097266

反应详情

EQUATION

反应方程式

HRID 2097266 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-(2,4-Bis-benzyloxy-5-chloro-phenyl)-4-(3-chloro-phenyl)-isoxazole-3-carboxylic acid ethylamide (36 mg, 0.06 mmol) in anhydrous THF under argon was added 1M Borane-THF complex (1 ml) and the solution refluxed overnight. After cooling the solution was poured on to a Isolute®SPE Flash SCX-2 5 g column which was quickly eluted with methanol (2×20 ml). The desired product was then recovered by eluting with a mixture of 10% ammonia in methanol (2×10 ml) which was evaporated in vacuo to provide 23 mg (65% yield) of a light yellow powder.

WORKUP

后处理

  1. temperaturethe solution refluxed overnight
  2. temperatureAfter cooling the solution
  3. additionwas poured on to a Isolute®SPE Flash SCX-2 5 g column which
  4. washwas quickly eluted with methanol (2×20 ml)
  5. customThe desired product was then recovered
  6. washby eluting with a mixture of 10% ammonia in methanol (2×10 ml) which
  7. customwas evaporated in vacuo