反应详情

Thiocyanic acid ammonium salt (10.6 g) was added to a mixture of 2-chloro-6-methyl-4-pyridinecarbonyl chloride (22.04 g; 116 mmol) and acetone (400 ml). The reaction mixture was stirred for 30 minutes and then 3,4-difluorobenzenamine (14.98 g; 116 mmol) was added slowly via an additional funnel. The resulting solution was stirred for 2 hours, quenched by water (100 ml) and then extracted by CH2Cl2 (3×100 ml). The combined organic phase was dried over MgSO4, filtered and the solvent was evaporated in vacuo. Yield: 38.1 g of intermediate D1.

1. stirringThe resulting solution was stirred for 2 hours
2. customquenched by water (100 ml)
3. extractionextracted by CH2Cl2 (3×100 ml)
4. dry with materialThe combined organic phase was dried over MgSO4
5. filtrationfiltered
6. customthe solvent was evaporated in vacuo