HRID452469
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of alkylated salt 2 (2.58 g, 9.65 mmol) in 20% aqueous NaOH solution (29.0 mmol) was heated at reflux for 16 h. The crude reaction mixture was evaporated to dryness and purified by silica gel column chromatography (CHCl3/MeOH, 10:1 (v/v), as eluent), to yield 3 (1.1 g, 93%) as a pale, brown powder; mp: 123-126° C. 1H NMR (CDCl3, 300 MHz) δ: 2.13 (s, 3H), 2.50 (s, 3H), 6.93 (s, 1H). Mass Spectrum: CI, m/z 124 (M+1).
WORKUP
后处理
- temperatureat reflux for 16 h
- customThe crude reaction mixture
- customwas evaporated to dryness
- custompurified by silica gel column chromatography (CHCl3/MeOH, 10:1 (v/v), as eluent)