HRID622596

反应详情

EQUATION

反应方程式

HRID 622596 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2,3-dihydro-2-methyl-1H-indole-7-sulfonamide (1.0 g) and (4-methoxy-6-methylpyrimidin-2-yl)carbamic acid methyl ester (1.0 g) in methylene dichloride (100 ml) was added trimethylaluminum (3.0 ml of a 2.0M solution in toluene). The mixture was heated at reflux for 18 hours under a nitrogen atmosphere. Work-up was achieved by careful addition of 100 ml of 1N HCl followed by separation of the organic layer. The methylene chloride was dried over MgSO4 and evaporated to dryness. The residue was chromatographed on a silica gel column to give the pure product (0.2 g, m.p. 175°-177° C.).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 18 hours under a nitrogen atmosphere
  3. customfollowed by separation of the organic layer
  4. dry with materialThe methylene chloride was dried over MgSO4
  5. customevaporated to dryness
  6. customThe residue was chromatographed on a silica gel column