Ethanol → HCID 178462187, compound

Participants

Reaction Steps

Analogously to Example 5, 514 mg (2.3 mmol) of N-benzyloxycarbonyl-(D/L)-alanine in 4.8 ml of THF and 506 μl (4.6 mmol) of NMM are activated with 349 1 (2.6 mmol) of isobutyl chloroformate and then reacted with 600 mg (2.3 mmol) of 3-amino-4-(3-chlorophenylamino)-1H-pyrazolo[3,4-d]pyrimidine (see Step 1.6). Dissolution of the crude product in 2 ml of DMSO at 100° C., addition of 30 ml of ethanol and cooling yield rac.-3-{(N-benzyloxycarbonyl-alanyl)-amino}-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine; mp. 238-240° C.; HPLC: tRet(grad20-100/20)=13.5; FAB-MS: (M+H)+=466.

Provenance & Evidence