反应详情

温度

80 °C

To 40 mg of 2-(4-bromophenyl)-N-(5-cyclopropyl-1H-pyrazol-3-yl)acetamide resin linked 1 ml of a 10.4M solution of CsF in DME:MeOH (3:1), phenylboronic acid (0, 12 mmol) in DME (0.5 ml) and tetrakis triphenylphosphine palladium, (Pd(PPh3)4, 0.008 mmol) in DME (1 ml) were added. The mixture was shaken 18 hrs at 80° C. and then washed with DMF (3×5 ml), MeOH (3×5 ml) and DCM (3×5 ml). To the resin 5 ml of TFA 10% in DCM were added and the mixture was shaken 1 hr at room temperature, the organic phase was filtered off and the resin was washed with DCM (3×5 ml) and DMSO (2×5 ml). The organic fractions were collected and evaporated under reduced pressure and the residue was analyzed by HPLC-MS (area count 90%, 254 nm; M+1=318, 2M+1=365) without further purification.

1. washwashed with DMF (3×5 ml), MeOH (3×5 ml) and DCM (3×5 ml)
2. additionTo the resin 5 ml of TFA 10% in DCM were added
3. stirringthe mixture was shaken 1 hr at room temperature
4. filtrationthe organic phase was filtered off
5. washthe resin was washed with DCM (3×5 ml) and DMSO (2×5 ml)
6. customThe organic fractions were collected
7. customevaporated under reduced pressure
8. customthe residue was analyzed by HPLC-MS (area count 90%, 254 nm; M+1=318, 2M+1=365) without further purification