反应详情

10 ml of a 50% solution of NH3 in MeOH were added to a solution of 0.9 g (2 mmol) of 3-benzenesulphonyl-7-chloro-2-methylsulphanyl-5-morpholin-4-ylmethyl-pyrazolo[1,5-a]pyrimidine in 20 DMF and stirred at RT for 4 hrs. The DMF was evaporated in a high vacuum and the residue was partitioned between 2N NaOH and CH2Cl2. The aqueous phase was extracted three times with CH2Cl2 and the combined organic phases were dried (MgSO4), filtered and evaporated. Subsequent chromatography (silica gel, CH2Cl2/MeOH/NH4OH 80:10:1) and crystallization from EtOH yielded 0.70 g (83%) of 3-benzenesulphonyl-5-(4-methyl-piperazin-1-ylmethyl)-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-7-ylamine as colorless crystals, m.p. 224-226°.

1. customThe DMF was evaporated in a high vacuum
2. customthe residue was partitioned between 2N NaOH and CH2Cl2
3. extractionThe aqueous phase was extracted three times with CH2Cl2
4. dry with materialthe combined organic phases were dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customSubsequent chromatography (silica gel, CH2Cl2/MeOH/NH4OH 80:10:1) and crystallization from EtOH