HRID38281

反应详情

EQUATION

反应方程式

HRID 38281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a vigorously stirred solution/suspension of the product from example 71 part a) (0.189 g) and solid sodium bicarbonate (0.215 g) in DCM (2 ml) and water (2 ml) was added phenylacetyl chloride (0.14 ml) dropwise. The mixture was stirred for 2 h. The organic layer and 1 further DCM extract were combined, dried (Na2SO4) and purified by passage through SCX resin eluting with MeCN, MeOH followed by 7M NH3 in MeOH. The basic fractions were concentrated in vacuo to give the sub-titled product as a white foam (0.205 g).

WORKUP

后处理

  1. extractionThe organic layer and 1 further DCM extract
  2. dry with materialdried (Na2SO4)
  3. custompurified by passage through SCX resin
  4. washeluting with MeCN, MeOH
  5. concentrationThe basic fractions were concentrated in vacuo