反应详情

A mixture of 4-chloro-3,5-dinitro-benzoic acid methyl ester (D25a) (2.6 g, 10 mmol, 1 equiv) and SnCl2 (18.95 g, 100 mmol, 10 equiv) in MeOH (80 ml) was refluxed for 1 h, cooled to room temperature and concentrated in vacuo. The residue was partitioned between AcOEt and 2N aqueous NaOH solution. The organic phase was dried over MgSO4 and concentrated in vacuo. The residue was triturated with 1:1 Et2O/iso-hexane to give 3,5-diamino-4-chloro-benzoic acid methyl ester (D27a) (1.56 g, 78%) as a light orange solid.

1. temperaturewas refluxed for 1 h
2. concentrationconcentrated in vacuo
3. customThe residue was partitioned between AcOEt and 2N aqueous NaOH solution
4. dry with materialThe organic phase was dried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was triturated with 1:1 Et2O/iso-hexane