反应详情

温度

20 °C

2,4-dichloro-7H-pyrrolo[2,3-d]pyrimidine (500 mg, 2.66 mmol), palladium(II)acetate (70 mg, 0.31 mmol) and BINAP (240 mg, 0.39 mmol) are dissolved in 6 mL THF and stirred for 20 min at 20° C. Then TMEDA (300 μL; 2.0 mmol) is added, the mixture is stirred for 20 min and then sodium borohydride (189 mg; 5.11 mmol) dissolved in 10 mL diglyme is added. After 1 h at 20° C. the mixture is combined with 1 N HCl and the solvent is eliminated in vacuo. The residue is purified by column chromatography (method prep. HPLC2; 3% acetonitrile to 55% in 12 min) and 2-chloro-7H-pyrrolo[2,3-d]pyrimidine (HPLC-MS: tRet.=1.25 min; MS(M+H)+=154; method FEC3) is obtained.

1. stirringthe mixture is stirred for 20 min
2. additionis added
3. customThe residue is purified by column chromatography (method prep. HPLC2; 3% acetonitrile to 55% in 12 min)