HRID1019404

反应详情

EQUATION

反应方程式

HRID 1019404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of 2-(4-methoxyphenyl)-4,4-dimethyl-2-oxazoline (11.0 g) in tetrahydrofuran (50 ml) is cooled to −50° C., and thereto is added dropwise a 1.6 M solution of n-butyl lithium in hexane (36.8 ml) over a period of 20 minutes. The mixture is stirred at 40° C. for 30 minutes, and thereto is added dropwise a solution of 3,4,5-trimethoxybenzaldehyde (10.5 g) in tetrahydrofuran (30 ml) at the same temperature over a period of 10 minutes. After reaction at −30T for one hour, to the mixture are added water and ethyl acetate. The ethyl acetate layer is separated, washed, dried, and concentrated under reduced pressure. The residue is crystallized from diethyl ether to give 2-{2-[hydroxy-(3,4,5trimethoxyphenyl)methyl]-4-methoxyphenyl}-4,4-dimethyl-2-oxazoline (16.2 g) as listed in Table 53.

WORKUP

后处理

  1. customAfter reaction at −30T for one hour
  2. customThe ethyl acetate layer is separated
  3. washwashed
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe residue is crystallized from diethyl ether