反应详情

To the solution of 0.58 g (1.25 mmol) 4-(2,4-dimethoxybenzylamino)-3-(5-nitro-4-thiocyanatopyrimidin-2-ylamino)benzonitrile in 10 mL 30% (v/v) TFA in DCM was added 0.01 mL of triethylsilane. The mixture was stirred for 0.5 hr. LCMS indicated the completion of de-protection. A red residue was obtained after removing the volatiles on rotary evaporator, and was suspended (majority dissolved) in 10 mL 1:1 trimethyl orthoformate: MeOH. The resulting mixture was stirred for 2 hrs at room temperature. Yellow solids were precipitated. Desired product (0.38 g, 95% overall yield) was obtained after suction filtration and washing with cold MeOH twice.

1. customA red residue was obtained
2. customafter removing the volatiles
3. customon rotary evaporator
4. dissolution(majority dissolved) in 10 mL 1:1 trimethyl orthoformate
5. stirringThe resulting mixture was stirred for 2 hrs at room temperature
6. customYellow solids were precipitated