反应详情

To a solution of crude 8-(4-amino-benzyl)-1,3-dimethyl-3,7-dihydro-purine-2,6-dione (0.2 mmol) in pyridine (2 mL) at 0° C. was added 5-chloro-1,3-dimethyl-1H-pyrazole-4-sulfonyl chloride (0.2 mmol) and the mixture left to stir and warm slowly to ambient temperature overnight. The reaction mixture was poured into ethyl acetate, washed with 1M aqueous hydrochloric acid until all pyridine was removed from the organic phase and the combined aqueous washings back extracted with ethyl acetate. The combined organic layers were dried and concentrated in vacuo to give an orange solid. Purified by trituration with warm acetonitrile to give 5-chloro-1,3-dimethyl-1H-pyrazole-4-sulfonic acid {4-[1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-amide as a pale orange solid (51%); EI-HRMS m/e calculated for C19H20ClN7O4S (M+) 477.0986, found 477.0994.

1. waitthe mixture left
2. washwashed with 1M aqueous hydrochloric acid until all pyridine
3. customwas removed from the organic phase
4. extractionthe combined aqueous washings back extracted with ethyl acetate
5. customThe combined organic layers were dried
6. concentrationconcentrated in vacuo
7. customto give an orange solid
8. customPurified by trituration with warm acetonitrile