HRID1730573

反应详情

EQUATION

反应方程式

HRID 1730573 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

28.9 gm (1.0 mol) of 2-acetonyl-3-oxo-naphth[2,1-d]isothiazoline-1,1-dioxide were added to a solution of 4.7 gm (2.04 gm-atom) of sodium in 125 ml of ethanol at 30° C. The resulting mixture was kept at 55° C for 2 hours, while stirring, and was subsequently refluxed for 15 minutes. After cooling, the reaction mixture was acidified with 350 ml of aqueous 9% hydrochloric acid, and the solid product formed thereby was suction-filtered off and washed with ice-cold 50% ethanol. Recrystallization from ethanol yielded 15.6 gm (54% of theory) of 3-acetyl-4-hydroxy-2H-naphtho[2,1-e]-1,2-thiazine-1,1-dioxide, m.p. 191°-192° C.

WORKUP

后处理

  1. temperaturewas subsequently refluxed for 15 minutes
  2. temperatureAfter cooling
  3. customthe solid product formed
  4. filtrationthereby was suction-filtered off
  5. washwashed with ice-cold 50% ethanol
  6. customRecrystallization from ethanol