反应详情

A solution of tris-dimethylaminophosphine in 2.6 mL of anhydrous THF was added under a nitrogen atmosphere to a solution of dibromodifluoromethane in 3.9 mL of anhydrous THF at 0° C. over 15 min. The reaction mixture was stirred at r.t. for 30 min. Afterwards, a solution of the Compound of Example 32 (0.275 g, 0.956 mmol) was added dropwise. After overnight resting, the solution was evaporated and taken up with EtOAc. Washing with water, drying the organic layer with Na2SO4 and evaporating to dryness in vacuo afforded a crude which was purified by means of automated flash chromatography (Isolera®TM-Biotage; gradient Petroleum Ether-EtOAc from 95:5 to 8:2) giving 42 mg of the title compound. Yield: 13.7%.

1. waitAfter overnight resting
2. customthe solution was evaporated
3. washWashing with water
4. dry with materialdrying the organic layer with Na2SO4
5. customevaporating to dryness in vacuo
6. customafforded a crude which
7. customwas purified by means of automated flash chromatography (Isolera®TM-Biotage; gradient Petroleum Ether-EtOAc from 95:5 to 8:2)