HRID427435

反应详情

EQUATION

反应方程式

HRID 427435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

4-(Naphthalene-2-sulphonyl)benzaldehyde (0.97 g) was suspended in water (25 ml) containing cetyltrimethylammonium bromide (58 mg). The mixture was stirred and heated to 60° C., and potassium permanganate (0.95 g) was added in small portions over 1 hour. Heating was continued for a further 2 hours. The mixture was cooled to room temperature and was acidified with 2M hydrochloric acid. Ethyl acetate was added to the stirred mixture, which was filtered through a pad of celite. The ethyl acetate layer was washed with brine, dried (MgSO4), and evaporated to afford 4-(naphthalene-2-sulphonyl)benzoic acid (0.42 g) as solid residue; NMR: 7.7(dd,1H); 7.95(dd,1H), 8.1-8.2(m,8H); 8.7(d,1H); microanalysis, found; C,58.6; H,3.9%; C17H12O4S.2H2O requires: C,58.6; H,4.6%; MS: m/z 312(M H)+.

WORKUP

后处理

  1. temperatureHeating
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationwas filtered through a pad of celite
  4. washThe ethyl acetate layer was washed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated