HRID439325

反应详情

EQUATION

反应方程式

HRID 439325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,3-diamino-5-fluorobenzoic acid (100 mg, 0.59 mmol) was combined with water (10 mL) in a small reaction vial. To this solution was slowly bubbled hydrogen chloride gas until all the solid dissolved, approximately 30 seconds. The solvents were removed in vacuo to produce a dark solid of 2,3-diamino-5-fluorobenzoic acid dihydrochloride (110 mg, 77%) which was identical in all respects to the sample prepared in Method A.: m.p. 215°-217° (dec); 1H NMR (400 MHz, D2O) δ 7.11 (dd, 1H), 7.43 (dd, 1H); 13C NMR (100 MHzD2O) δ 102.4, 102.7, 104.6, 104.8, 109.3, 109.4, 137.0, 138.5, 138.6, 152.0, 154.8, 170.1.

WORKUP

后处理

  1. dissolutiondissolved, approximately 30 seconds
  2. customThe solvents were removed in vacuo