HRID224952

反应详情

EQUATION

反应方程式

HRID 224952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.63 grams of 2-bromohexanoic acid methyl ester, 8.52 grams of potassium cyanate and 7.85 grams of methanol were heated in 70 ml of dimethylformamide (DMF) at 100° C. for 45 minutes under vigorous stirring. After the cooling off of the reaction mixture the salts were filtered off and the filtrate concentrated in a vacuum. The viscous residue was taken up with 50 ml of acetone and the undissolved material filtered off. Subsequently the acetone was distilled off and the residue fractionated in the high vacuum. There resulted 10.75 grams (75.5%) of 2-methoxycarbonylaminohexanoic acid methyl ester having a boiling point of 78° C./0.007 mbar.

WORKUP

后处理

  1. filtrationAfter the cooling off of the reaction mixture the salts were filtered off
  2. concentrationthe filtrate concentrated in a vacuum
  3. filtrationthe undissolved material filtered off
  4. distillationSubsequently the acetone was distilled off