反应详情

In 4 ml of THF/DMEU 1:3, 40 mg (0.08 mmol) of rac.-3-([N-benzyloxycarbonylvalyl]-amino)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine (see Example 8) are hydrogenated in the presence of 10 mg of Pd/C (10%) and 10 μl of 1,2-dichlorobenzene. The catalyst is filtered off, and the filtrate is partially concentrated by evaporation in a rotary evaporator, poured into 30 ml of water and again filtered and the filtrate is concentrated by evaporation under a high vacuum first at RT and finally at 50° C. to yield rac.-4-(3-chlorophenylamino)-3-(valyl-amino)-1H-pyrazolo[3,4-d]pyrimidine; HPLC: tRet(grad20-100/20)=9.2; FAB-MS: (M+H)+=360.

1. filtrationThe catalyst is filtered off
2. concentrationthe filtrate is partially concentrated by evaporation in a rotary evaporator
3. additionpoured into 30 ml of water
4. filtrationagain filtered
5. concentrationthe filtrate is concentrated by evaporation under a high vacuum first at RT and finally at 50° C.