HRID2374674

反应详情

EQUATION

反应方程式

HRID 2374674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 2,3-diaminobenzamide dihydrochloride (synthesized as described in U.S. Pat. No. 6,737,421, column 11, EXAMPLE 2, step (e), 5 g, 22.3 mmol) and 4-bromobenzaldehyde (4.13 g, 22.3 mmol) in methanol (200 mL) was added 10% Pd/C (1.3 g). The mixture was refluxed overnight, then cooled and filtered though a pad of celite. The filtrate was concentrated under vacuum and purified by chromatography on a silica gel column with 0-10% methanol/dichloromethane to provide the title compound (1.2 g, 17%). MS (ESI) m/e 317 (M+H)+.

WORKUP

后处理

  1. customsynthesized
  2. temperatureThe mixture was refluxed overnight
  3. temperaturecooled
  4. filtrationfiltered though a pad of celite
  5. concentrationThe filtrate was concentrated under vacuum
  6. custompurified by chromatography on a silica gel column with 0-10% methanol/dichloromethane