HRID59048

反应详情

EQUATION

反应方程式

HRID 59048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-methyl-4H-benzo[d][1,3]oxazin-4-one (101 mg, 0.63 mmol) and 1-(3-aminophenyl)-1,4-dihydro-5H-tetrazol-5-one (111 mg, 0.63 mmol) in AcOH (10 mL) was heated to reflux and stirred overnight. Analysis indicated the formation of product. The mixture was allowed to cool and dry-loaded onto silica gel. The mixture was purified by column chromatography on silica gel using CH2Cl2/MeOH (1:0 to 9:1) as eluent to give the product (32 mg, 16% ca. 94% purity by LC/MS). The product was used directly in the next step.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux
  3. temperatureto cool and dry-loaded onto silica gel
  4. customThe mixture was purified by column chromatography on silica gel
  5. customto give the product (32 mg, 16% ca. 94% purity by LC/MS)