HRID267354

反应详情

EQUATION

反应方程式

HRID 267354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.2 g. (3.24 mmole) of 1-hydroxy-3-(3-methyl-2-octyl)-7,8,9,10-tetrahydro-6,6,10-trimethyl-6H-dibenzo[b,d]pyran, 0.73 g. (3.24 mmole) of 2-methyl-4-morpholinobutyric acid hydrochloride, 0.71 g. (3.46 mmole) of dicyclohexylcarbodiimide and 50 ml. of methylene chloride was stirred at room temperature for 16 hrs. The reaction mixture was cooled and the byproduct of dicyclohexylurea was removed by filtration. The solvent was evaporated to give a foamy residue which was chromatographed using activated magnesium silicate and methanol/chloroform solvent mixtures. The fractions were monitored by thin layer chromatography and the desired material was obtained from the 2% methanol/chloroform fractions. The appropriate fractions were collected and evaporated to give 0.9 g. (51%) of light purple gum.

WORKUP

后处理

  1. additionA mixture of 1.2 g
  2. temperatureThe reaction mixture was cooled
  3. customthe byproduct of dicyclohexylurea was removed by filtration
  4. customThe solvent was evaporated
  5. customto give a foamy residue which
  6. customwas chromatographed