HRID866880

反应详情

EQUATION

反应方程式

HRID 866880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(2,4-Dinitrophenylthio)-1-(2-methanesulfonamidoethyl)tetrazole (4.46 g, 11.5 mmol) was added to 60 ml of 5% sodium methoxide in methanol. After 1 hour, water was added and the solid material was removed by filtration. The filtrate was concentrated in vacuo and 3N hydrochloric acid was added to the residue to bring the pH to 1.4. The acidic solution was filtered and the filtrate was extracted twice with ethyl acetate. The extracts were combined and concentrated to give a residue which crystallized upon addition of ethyl acetate to give 1-(2-methanesulfonamidoethyl)tetrazole-5-thiol, mp 131°-132°.

WORKUP

后处理

  1. customthe solid material was removed by filtration
  2. concentrationThe filtrate was concentrated in vacuo and 3N hydrochloric acid
  3. additionwas added to the residue
  4. filtrationThe acidic solution was filtered
  5. extractionthe filtrate was extracted twice with ethyl acetate
  6. concentrationconcentrated
  7. customto give a residue which
  8. customcrystallized upon addition of ethyl acetate