HRID439325
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- dissolutiondissolved, approximately 30 seconds
- customThe solvents were removed in vacuo