反应详情

To a stirring solution of methyl 2,3-diamino-4-(trifluoromethyl)benzoate (5.10 g, 0.022 mol) and diisopropylethylamine (6.26 g, 0.048 mol) in toluene (50 ml) was added a solution of triphosgene (2.58 g, 0.0087 mol) in toluene (20 ml) dropwise and stirred at room temperature for 16 h. The reaction mixture was concentrated in vacuo. The residue was diluted with 1N hydrochloric acid and extracted with ethyl acetate and tetrahydrofuran. The extracts were washed with water, dried over magnesium sulfate and concentrated in vacuo. A solution of 50% diisopropylether/n-hexane was added to the residue and white precipitates were filtered, washed with same solvent to give 5.00 g (0.019 mol 87%) of the title as a white powder

1. concentrationThe reaction mixture was concentrated in vacuo
2. additionThe residue was diluted with 1N hydrochloric acid
3. extractionextracted with ethyl acetate and tetrahydrofuran
4. washThe extracts were washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. additionA solution of 50% diisopropylether/n-hexane was added to the residue
8. customwhite precipitates
9. filtrationwere filtered
10. washwashed with same solvent
11. customto give 5.00 g (0.019 mol 87%) of the title as a white powder