反应详情

A solution of tert-butyl 3-(5-amino-6-(dibenzylamino)pyrimidin-4-ylamino)phenylcarbamate (3) (4.0 g, 8.1 mmol) and TEA (2 mL, 14.5 mmol) in 80 mL dry DCM was cooled to 0° C. under N2, triphosgene (1.2 g, 4.0 mmol) in 10 mL dry DCM was added dropwise during 2 hrs. After additional 1 hr stirring, the reaction was quenched with water (100 mL). The organic layer was separated, washed with water (100 mL×2) and brine (100 mL×1), dried over Na2SO4, then concentrated to dryness in vacuo. tert-Butyl 3-(6-(dibenzylamino)-8-oxo-7H-purin-9(8H)-yl)phenylcarbamate (4) (3.0 g, 71%) was obtained as a brown solid. LC-MS (ESI): m/z (M+1) 523.

1. customthe reaction was quenched with water (100 mL)
2. customThe organic layer was separated
3. washwashed with water (100 mL×2) and brine (100 mL×1)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to dryness in vacuo