反应详情

To a solution of [3-({5-nitro-4-[(4-pyrrolidin-1-yl-cyclohexylmethyl)-amino]-pyrimidin-2-ylamino}-methyl)-benzyl]-carbamic acid tert-butyl ester (132 mg, 0.25 mmol) in DCM (1 mL) was added TFA (2 mL). After 20 min the reaction mixture was concentrated in vacuo and the resulting oil taken up in EtOAc and the solution washed with sat. NaHCO3. The aqueous layer was then extracted with 90:10 CHCl3/i-PrOH. The combined organic layers were concentrated in vacuo and the residue purified by column chromatography (silica gel, 96:4 to 93:7 DCM/10% NH4OH in MeOH) to afford the title compound (25 mg), m/z 440 (M+1)+.

1. concentrationAfter 20 min the reaction mixture was concentrated in vacuo
2. washthe solution washed with sat. NaHCO3
3. extractionThe aqueous layer was then extracted with 90:10 CHCl3/i-PrOH
4. concentrationThe combined organic layers were concentrated in vacuo
5. customthe residue purified by column chromatography (silica gel, 96:4 to 93:7 DCM/10% NH4OH in MeOH)