HRID426284

反应详情

EQUATION

反应方程式

HRID 426284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(7-Hydroxy-2,4-dimethoxy-5,5-dimethyl-5,7-dihydro-furo[3,4-d]pyrimidin-7-yl)-5-methyl-benzonitrile (0.027 g, 0.080 mmol) in acetyl bromide (2.0 mL) was heated at 60° C. for 3 h. Reaction mixture was concentrated and purified by reverse phase HPLC (Phenomenex Synergi® column, 5 to 100% acetonitrile/H2O) to give a desired product (0.0063 g, 25%). 1H NMR (300 MHz, CD3OD): δ 7.76 (s, 1H), 7.70 (s, 1H), 7.51 (s, 1H), 2.38 (s, 1H), 1.60 (s, 3H), 1.59 (s, 3H). Mass spectrum: 314.0 (M+H)+.

WORKUP

后处理

  1. customReaction mixture
  2. concentrationwas concentrated
  3. custompurified by reverse phase HPLC (Phenomenex Synergi® column, 5 to 100% acetonitrile/H2O)