HRID1062498

反应详情

EQUATION

反应方程式

HRID 1062498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a stirring solution of 2,6-Dimethylquinaldine (1) (5 g, 0.0318 mol) in 1,2 dichloroethane (130 ml) was added 3-CPBA (3-chloro-peroxybenzoic acid) (7.43 g of 72% activity, 0.0310 mol). The reaction was then heated to 40° C. for 24 hours. The completed reaction mixture was allowed to cool to room temperature, concentrated, and 10% K2CO3 and a minimal amount of ethyl acetate was to produce a two phase mixture. A precipitate then formed in both layers and was filtered, washed with water to remove traces of K2CO3 and dried to afford 4.67 g (85%). H1 NMR (CDCl3): δ 2.52_(s, 3H), 2.66 (s, 3H), 7.28-7.56 (m, 4H), 8.70-8.79 (m, 1H).

WORKUP

后处理

  1. customThe completed reaction mixture
  2. temperatureto cool to room temperature
  3. concentrationconcentrated
  4. customto produce a two phase mixture
  5. customA precipitate then formed in both layers
  6. filtrationwas filtered
  7. washwashed with water
  8. customto remove traces of K2CO3
  9. customdried
  10. customto afford 4.67 g (85%)