反应 #10827

反应方程式

hydrazine

2,4-dimethoxy-benzoic acid methyl ester

→

2,4-dimethoxy-benzoic acid hydrazide

收率 78.1%

溶剂

methanol

反应条件

后处理

1. 1
   其他Solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONThe residue was re-dissolved in ethyl acetate
3. 3
   洗涤The solution of ethyl acetate was washed with saturated solution of sodium bicarbonate and brine
4. 4
   干燥dried over sodium carbonate
5. 5
   浓缩concentrated

实验过程

Ex-109A: A solution of 2,4-dimethoxy-benzoic acid methyl ester (4.24 g, 21.6 mmol) and hydrazine (3.4 mL, 108.1 mmol) in methanol (50 mL) was refluxed overnight. Solvent was removed under reduced pressure. The residue was re-dissolved in ethyl acetate. The solution of ethyl acetate was washed with saturated solution of sodium bicarbonate and brine, dried over sodium carbonate and concentrated to afford 2,4-dimethoxy-benzoic acid hydrazide (3.31 g, 78%) as a white solid: 1H NMR (CDCl3) δ 8.77 (bs, 1H), 8.15 (d, J=8.8 Hz, 1H), 6.58 (dd, J=8.8, 2.2 Hz, 1H), 6.46 (d, J=2.2 Hz, 1H), 4.10 (bs, 2H), 3.91 (s, 3H), 3.83 (s, 3H).

来源