Trifluoroacetic acid → 6-(2-Amino-ethyl)-5-(3-chloro-phenyl)-1,3-dimethyl-1,6-dihydro-pyrrolo[3,4-d]pyrimidine-2,4-dione
反応式
C(OC(=O)[NH:7][CH2:8][CH2:9][N:10]1[C:18]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)=[C:17]2[C:12]([N:13]([CH3:29])[C:14](=[O:28])[N:15]([CH3:27])[C:16]2=[O:26])=[CH:11]1)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:7][CH2:8][CH2:9][N:10]1[C:18]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)=[C:17]2[C:12]([N:13]([CH3:29])[C:14](=[O:28])[N:15]([CH3:27])[C:16]2=[O:26])=[CH:11]1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
{2-[5-(3-Chloro-phenyl)-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydro-pyrrolo[3,4-d]pyrimidin-6-yl]-ethyl}-carbamic acid tert-butyl ester (step 5) (429 mg, 0.991 mmol) was dissolved in DCM (10 ml). TFA (1.374 ml, 17.84 mmol) was charged in 2 portions and the reaction stirred under nitrogen. After 2 hrs, the pH of the mixture was adjusted to pH 11 with saturated K3CO3 solution (20 mL). The layers were separated and the aqueous extracted with DCM (4×20 mL). The combined organics were passed through a hydrophobic frit and evaporated under reduced pressure to afford a tan solid, which was dried under vacuum at 50° C. for 5 h to afford the title compound as a tan solid.