HRID746043

反应详情

EQUATION

反应方程式

HRID 746043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,6-dichloro-4-nitrotoluene (2.0 g 9.7 mmol) in tetrahydrofuran: methanol mixture (20:11 cm3) was added slowly to a vigorously stirred solution of 10-14% aqueous sodium hypochlorite (15 cm3) at 0° C. After 3.75 h at this temperature, the mixture was poured into dilute hydrochloric acid and then extracted with chloroform (30 cm3). The organic extract was dried and evaporated to yield an organge oil which was purified by flash chromatography over silica gel eluting with an ethyl acetate-petroleum ether gradient. The title compound was obtained as a pale orange solid, m.p. 37°-9° C. (1.8 g).

WORKUP

后处理

  1. extractionextracted with chloroform (30 cm3)
  2. extractionThe organic extract
  3. customwas dried
  4. customevaporated
  5. customto yield an organge oil which
  6. customwas purified by flash chromatography over silica gel eluting with an ethyl acetate-petroleum ether gradient