反应详情

To 4-(3-ethynyl-phenylamino)-7H-pyrrolo[2,3-d]pyrimidine-5-carboxylic acid (0.108 g, 0.39 mmol) in dry methylene chloride (2 ml) was added a solution of oxalyl chloride (0.17 ml, 1.9 mmol) in dry methylene chloride (4 ml) followed by 1 drop of dry DMF. The suspension was stirred at ambient temperature for 1 hour, then concentrated in vacuo. To the resulting solid was added dry acetone (2 ml) and dry methanol (1 ml). The solution was stirred at ambient temperature for 15 hours, then concentrated in vacuo. The residue was diluted with ethyl acetate and water, and the solid filtered and dried in vacuo to afford the title compound as a tan powder (40 mg, 35%). TS-MS: 293 (MH+); anal. RP18-HPLC RT: min.

1. concentrationconcentrated in vacuo
2. additionTo the resulting solid was added dry acetone (2 ml) and dry methanol (1 ml)
3. stirringThe solution was stirred at ambient temperature for 15 hours
4. concentrationconcentrated in vacuo
5. additionThe residue was diluted with ethyl acetate and water
6. filtrationthe solid filtered
7. customdried in vacuo