HRID129997

反应详情

EQUATION

反应方程式

HRID 129997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(1,3-Dithiol-2-ylidene)malonic acid dimethyl ester (232 mg) prepared according to the procedure described in JP-76.48666, was suspended in methanol (0.1 ml) and 1N KOH/methanol (3.0 ml) was added. The reaction mixture was refluxed for 1 h and then concentrated under reduced pressure. The residue was dissolved in water and the pH of the solution was adjusted to 2 with 1N HCl. The resulting precipitate was collected by filtration, washed with water, and dried in vacuo to give the title compound (196 mg) as a pale yellow powder.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 1 h
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water
  6. customdried in vacuo