HRID2166039

反应详情

EQUATION

反应方程式

HRID 2166039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 36.5 parts of 1-butyl-1H-benzotriazole-5-methanol, 35 parts of manganese(IV) oxide and 390 parts of dichloromethane was stirred for 12 hours at room temperature. The manganese(IV) oxide was filtered off over diatomaceous earth and another portion of 35 parts of manganese(IV) oxide was added to the filtrate. After stirring for 12 hours at room temperature, the whole was filtered and the filtrate was evaporated. The residue was purified by column chromatography over silica gel using dichloromethane as eluent. The pure fractions were collected and the eluent was evaporated, yielding 15.3 parts (42.2%) of 1-butyl-1H-benzotriazole-5-carboxaldehyde as a residue (int. 57).

WORKUP

后处理

  1. filtrationThe manganese(IV) oxide was filtered off over diatomaceous earth
  2. additionanother portion of 35 parts of manganese(IV) oxide was added to the filtrate
  3. stirringAfter stirring for 12 hours at room temperature
  4. filtrationthe whole was filtered
  5. customthe filtrate was evaporated
  6. customThe residue was purified by column chromatography over silica gel
  7. customThe pure fractions were collected
  8. customthe eluent was evaporated