反应详情

An ice-cold solution of phosgene (1.1 M solution in toluene; 0.91 ml) was diluted with CH2Cl2 (3 ml) and then a solution of 56 (0.34 g, 1.0 mmol) and triethylamine (0.28 ml; 2.0 mmol) in CH2Cl2 (3 ml) was added slowly with cooling (ice-bath). Then a solution of 57 (0.25 g; 1.0 mmol) and triethyl amine (0.14 ml; 1.0 mmol) in CH2Cl2 (3 ml) was added and stirring was continued at room temperature for 6 hours. The reaction mixture was diluted with EtAc (25 ml) and extracted with H2O (2×10 ml) and brine, and dried (MgSO4). The residue after evaporation was subjected to chromatography on silica gel, allowing isolation of 58.

1. temperaturewith cooling (ice-bath)
2. additionThe reaction mixture was diluted with EtAc (25 ml)
3. extractionextracted with H2O (2×10 ml) and brine
4. dry with materialdried (MgSO4)
5. customThe residue after evaporation