反应详情

Under a nitrogen atmosphere, 320 μl (2.9 mmol) of NMM and 210 1 (1.6 mmol) of isobutyl chloroformate are added at −20° C. to 250 mg (1.5 mmol) of 2,3-methylenedioxybenzoic acid [for preparation see: Chem. Ber. 104 (1971) 2347] in 3.2 ml of THF and then stirred for 45 min. 378 mg (1.45 mmol) of 3-amino-4-(3-chloro-phenylamino)-1H-pyrazolo-[3,4-d]pyrimidine (see Step 1.6) are then added and the reaction mixture is allowed to rise to RT and is stirred for 1 hour to complete the reaction. The reaction mixture is poured into 100 ml of water and stirred for 1 hour, and the crude product is filtered off and washed with water and ethanol. Dissolution in 3 ml of DMSO at =110° C., cooling, filtering and washing with ethanol yield 4-(3chloro-phenylamino)-3-(2,3-methylenedioxy-benzoylamino)-1H-pyrazolo[3,4-d]pyrimidine; HPLC:tRet(grad20-100/20)=16.5; FAB-MS: (M+H)+=409.

1. customto rise to RT
2. stirringis stirred for 1 hour
3. customthe reaction
4. stirringstirred for 1 hour
5. filtrationthe crude product is filtered off
6. washwashed with water and ethanol
7. dissolutionDissolution in 3 ml of DMSO at =110° C.
8. temperaturecooling
9. filtrationfiltering
10. washwashing with ethanol