HRID580953

反应详情

EQUATION

反应方程式

HRID 580953 的结构方程式

PROCEDURE

实验过程

A solution of ethyl 4-allyloxyphenoxyacetate (2.0 g) in diphenylether (15 ml) was heated at reflux for 12 minutes. The reaction mixture was allowed to cool to ambient temperature and the reaction mixture was poured onto a silica gel pad (Merck Art. No. 9385). Elution with hexane followed by a 4:1 (v/v) mixture of hexane and ethyl acetate gave ethyl 3-allyl-4-hydroxyphenoxyacetate (1.62 g) as a solid, mp 52.8° C.; microanalysis, found: C, 66.3; H, 7.20%; C13H16O4 requires: C, 66:1; H, 6.83%; NMR (CDCl3): 1.28 (3H, t), 3.35 (2H, d), 4.25 (2H, q), 4.55 (2H, s), 4.73 (1H, s), 5.07-5.20 (2H, m), 5.88-6.10 (1H, m) and 6.62-6.78 (3H, m); m/z 237 (M+H).

WORKUP

后处理

  1. temperatureat reflux for 12 minutes
  2. additionthe reaction mixture was poured onto a silica gel pad (Merck Art
  3. washElution with hexane
  4. additionfollowed by a 4:1 (v/v) mixture of hexane and ethyl acetate