HRID258669

反应详情

EQUATION

反应方程式

HRID 258669 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Methoxyquinaldic acid (7.25 g) was dissolved in dry dimethylformamide (20 ml). N,N'-carbonyldiimidazole (5.8 g) was added, and the solution was stirred for 6 hours at room temperature. 5-Aminotetrazole (3.69 g) was added and the mixture was stirred overnight at room temperature. The solid was filtered off, washed with methanol and dissolved in dimethylformamide (50 ml) with the minimum addition of dimethylaminoethanol to effect dissolution. Water (50 ml) was added, and the solution was adjusted to pH 2 by the addition of aqueous hydrochloric acid. The solid was filtered off to give 4-methoxy-N(1H-tetrazol- 5-yl)quinaldamide, m.p. 289° (d).

WORKUP

后处理

  1. stirringthe mixture was stirred overnight at room temperature
  2. filtrationThe solid was filtered off
  3. washwashed with methanol
  4. dissolutiondissolved in dimethylformamide (50 ml) with the minimum addition of dimethylaminoethanol
  5. dissolutiondissolution
  6. additionWater (50 ml) was added
  7. additionthe solution was adjusted to pH 2 by the addition of aqueous hydrochloric acid
  8. filtrationThe solid was filtered off