HRID838902

反应详情

EQUATION

反应方程式

HRID 838902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-(1-naphthyl)acrylic acid (50.0g., 0.25 moles) in concentrated hydrochloric acid (1500 ml.) was stirred at reflux while a vigorous stream of hydrogen chloride was passed through the reaction for 6 hours. The solution was allowed to stand overnight at room temperature, then filtered to give a white solid which was dissolved in ethyl acetate and washed with saturated sodium bicarbonate solution (3×). The ethyl acetate solution was dried and removal of solvent gave the dihydrocoumarin as a white solid (43.5g., 85% based on consumed starting material) m.p. 193°-196° C.

WORKUP

后处理

  1. customwas passed through the reaction for 6 hours
  2. filtrationfiltered
  3. customto give a white solid which
  4. washwashed with saturated sodium bicarbonate solution (3×)
  5. dry with materialThe ethyl acetate solution was dried
  6. customremoval of solvent
  7. customgave
  8. customthe dihydrocoumarin as a white solid (43.5g., 85% based on consumed starting material) m.p. 193°-196° C.