反应详情

2-Amino-4,6-dichloropyrimidine (6.15 g, 0.0375 mol) is added portionwise to a solution of chlorosulfonyl isocyanate (5.30 g, 0.0375 mol) in methylene chloride at 0° C. The resulting mixture is stirred at 0° to 2° C. for two hours and a solution of o-aminophenyl cyclopropyl ketone (6.04 g, 0.0375 mol) and triethylamine (3.8 g, 0.0406 mol) in methylene chloride is slowly added to the mixture. The resulting solution is stirred at room temperature overnight, washed with water, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain the title product as a yellow solid (14.3 g, 75% real by HPLC analysis, 68% yield) which is used as a starting material for Example 2 without purification. A portion of the yellow solid is purified to yield the title product, mp 114°-116° C.

1. stirringThe resulting solution is stirred at room temperature overnight
2. washwashed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo