HRID231044

反应详情

EQUATION

反应方程式

HRID 231044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 25 ml of DMF was added methyl iodide (2.9 ml), 4-chloro-3-hydroxy-10H-phenothiazine (see Example 3) (2.3 g) and sodium hydride (0.672 g). The resulting reaction mixture was stirred at ambient temperature for 12 hours. At 0° C., MeOH was added to destroy the remaining hydride, then H2O. The resulting solution was extracted with ethyl acetate and the organic phase, dried and evaporated. The resulting residue was then purified by chromatography on silica gel to give 1.5 g of 4-chloro-3-methoxy-10-methyl-10H-phenothiazine (m.p.: 136° C.).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. customto destroy the remaining hydride
  3. extractionThe resulting solution was extracted with ethyl acetate
  4. customthe organic phase, dried
  5. customevaporated
  6. customThe resulting residue was then purified by chromatography on silica gel