HRID638700

反应详情

EQUATION

反应方程式

HRID 638700 的结构方程式

PROCEDURE

实验过程

To a solution of methanol (2100 ml) and sulphuric acid (84 ml) was added 2-(6-Hydroxynaphthalen-2-yl)-propionic acid 5 (420 g, 1.944 mmol), and refluxed for 6 hours. Methanol (1000 ml) was distilled off and the cooled reaction mass was poured onto ice water (3000 ml). Crude 6 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 6 (400 g, 89.5%) as a white fluffy powder. The melting point found to be 89.5-92° C. The structure was confirmed with IR and NMR.

WORKUP

后处理

  1. temperaturerefluxed for 6 hours
  2. distillationMethanol (1000 ml) was distilled off
  3. customthe cooled reaction mass
  4. additionwas poured onto ice water (3000 ml)
  5. filtrationCrude 6 was filtered
  6. customdried
  7. customrecrystallised from a mixture of ethyl acetate:hexane (1:5)