反应详情

A mixture of 3-nitro-5-trifluoromethyl-phenol (750 mg, Step C), K2CO3 (3 eq., 1.5 g) and 3-hydroxymethyl-azetidine-1-carboxylic acid benzyl ester (1.1 eq., 1.2 g) in DMF was heated to 80 C for 1 h. The solution was cooled to RT then filtered and concentraced under vacuum. The residue was dissolved in CH2Cl2 and washed with H2O twice, followed by brine. The organic layer was dried over Na2SO4 and evaporated under reduced pressure. The residue was purified by column chromatography using 5% MeOH/CH2Cl2 to provide the desired compound as a colorless solid.

1. temperaturewas heated to 80 C for 1 h
2. filtrationthen filtered
3. dissolutionThe residue was dissolved in CH2Cl2
4. washwashed with H2O twice
5. dry with materialThe organic layer was dried over Na2SO4
6. customevaporated under reduced pressure
7. customThe residue was purified by column chromatography