反应详情

To a solution of 1-methyl-4,5,6,7-tetrahydro-1H-indazol-4-ol (400 mg, 2.63 mmol) and 3-iodo-1H-pyrazolo[3,4-d]pyrimidin-4-amine (684 mg, 2.63 mmol) and Ph3P (1.03 g, 3.94 mmol) in THF (40 mL) was added DIAD (798 mg, 3.94 mmol) dropwise at 0° C. After the addition was completed, the mixture was allowed to warm to room temperature and stirred for 3 hours. The mixture was extracted with EA, the combined the organic layers were washed with brine and dried over anhydrous Na2SO4. The volatiles were concentrated in vacuo and the residue was purified by silica gel chromatography (DCM/methanol=40/1 v/v %) to give 3-iodo-1-(1-methyl-4,5,6,7-tetrahydro-1H-indazol-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (80 mg, 8%). MS-ESI (m/z): 396 (M+1)+ (Acq Method: 10-80AB_2 min_220 &254.1 cm; Rt: 0.82 min)

1. additionAfter the addition
2. extractionThe mixture was extracted with EA
3. washwere washed with brine
4. dry with materialdried over anhydrous Na2SO4
5. concentrationThe volatiles were concentrated in vacuo
6. customthe residue was purified by silica gel chromatography (DCM/methanol=40/1 v/v %)