HRID1484011

反应详情

EQUATION

反应方程式

HRID 1484011 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Cocrystals of dimethyl fumarate and (+)-camphoric acid were prepared as follows. 36 mg of dimethyl fumarate and 200 mg of (+)-camphoric acid were combined in an agate jar with a 4 ml capacity. One drop of 1:3 (v:v) ethyl acetate:heptane was added along with two agate grinding balls. The mixture was milled for 60 minutes at full power on a Retch mm2 mixer mill. The starting concentrations of dimethyl fumarate and (+)-camphoric acid were chosen such that the thermodynamically stable solid phase at equilibrium is the cocrystal of dimethyl fumarate and (+)-camphoric acid. The crystalline material that formed was isolated to yield the dimethyl fumarate: (+)-camphoric acid (1:4, by NMR) cocrystal. The measured melting points were 103±1° C. for dimethyl fumarate, 185±2° C. for (+)-camphoric acid, and 88±2° C. for the cocrystal.

WORKUP

后处理

  1. customgrinding balls
  2. customThe mixture was milled for 60 minutes at full power on a Retch mm2 mixer mill
  3. customThe crystalline material that formed
  4. customwas isolated