反应详情

To a solution of 3.7 g (12.5 mmol) of triphosgene in THF at 0° C. was added dropwise a mixture of 2.5 g (6.2 mmol) of amine 1-8 and 1.74 mL (12.5 mmol) of triethylamine in THF. The reaction was allowed to warm to room temperature overnight with stirring. The mixture was then dumped into water, placed in a separatory funnel, and extracted twice with EtOAc. The combined organic extracts were combined, washed with water, dried over Na2SO4 and concentrated to obtain 6-1 as a brown solid. Data for 6-1: HRMS (ES) calc'd M+H for C24H28ClF2NO2Si: 464.1619. Found: 464.1625.

1. customplaced in a separatory funnel
2. extractionextracted twice with EtOAc
3. washwashed with water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated