HRID638700
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturerefluxed for 6 hours
- distillationMethanol (1000 ml) was distilled off
- customthe cooled reaction mass
- additionwas poured onto ice water (3000 ml)
- filtrationCrude 6 was filtered
- customdried
- customrecrystallised from a mixture of ethyl acetate:hexane (1:5)