HRID963476

反应详情

EQUATION

反应方程式

HRID 963476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 4-nitro-2-picoline-1-oxide (0.952 g) in dry methanol (20 ml) was added dropwise a solution of sodium methox-ide prepared from sodium (0.60 g) and methanol (10 ml) under stirring at cooling in an ice-bath. The mixture was stirred for 3 hours under the same condition. The resultant mixture was concentrated in vacuo. The residue was treated with chloroform and water. The organic layer was washed with water and a brine, and dried over sodium sulfate. Removal of the solvent gave 4-methoxy-2-picoline-1-oxide (0.958 g).

WORKUP

后处理

  1. temperatureat cooling in an ice-bath
  2. stirringThe mixture was stirred for 3 hours under the same condition
  3. concentrationThe resultant mixture was concentrated in vacuo
  4. additionThe residue was treated with chloroform and water
  5. washThe organic layer was washed with water
  6. dry with materiala brine, and dried over sodium sulfate
  7. customRemoval of the solvent