反应详情

Dimethylsulfamoyl chloride (7.2 g, 0.05 mole) was added dropwise to a solution of 2-hydroxyethyl 5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrobenzoate (10 g, 0.025 mole), triethylamine (10 ml) and ethyl ether (200 ml). The mixture was heated to and held at reflux for 5 hrs., cooled, added 200 ml of ether and washed three times with water. The ethereal solution was dried over MgSO4, concentrated to 13.9 g of yellow gum. The gummy material was run through a silica gel with 30% acetone-70% cyclohexane as eluent to afford 3.0 g of pure 2-(N,N-dimethylsulfamoyloxy)ethyl 5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrobenzoate as colorless gum; nmr (CDCl3) 2.96 (S, 6H), 3.84 (m, 2H), 4.52 (m, 2H), 6.88-8.24 (m, 6H).

1. temperatureThe mixture was heated to and
2. temperatureat reflux for 5 hrs
3. temperature, cooled
4. washwashed three times with water
5. dry with materialThe ethereal solution was dried over MgSO4
6. concentrationconcentrated to 13.9 g of yellow gum