反应详情

92 mg of NaH (65%) were added at room temperature to a solution of 162.5 mg of 4-amino-6-methoxy-5-(2-methoxy-phenoxy)-2,2'-bipyrimidine in 10 ml of tetrahydrofuran, the solution was stirred at room temperature for 11/2 hours and subsequently 162.5 mg of 5-tert-butyl-thiophene-2-sulphonyl chloride were added at the same temperature. The mixture was stirred at room temperature for a further 2 hours, poured on to ice/water, extracted with ethyl acetate, the aqueous phase was acidified and extracted with methylene chloride. The combined, organic phases were dried over magnesium sulphate and concentrated on a rotary evaporator. The residue was chromatographed over silica gel with methylene chloride/methanol (20/1) as the eluent. 5-tert-Butyl-N-[6-methoxy-5-(2-methoxy-phenoxy)-2,2'-bipyrimidin-4-yl]-thiophene-2-sulphonamide was obtained as a yellow powder. MS: 463 (M-SO2).

1. additionwere added at the same temperature
2. extractionextracted with ethyl acetate
3. extractionextracted with methylene chloride
4. dry with materialorganic phases were dried over magnesium sulphate
5. concentrationconcentrated on a rotary evaporator
6. customThe residue was chromatographed over silica gel with methylene chloride/methanol (20/1) as the eluent