反应详情

A suspension of 1.3 g (3.43 mmol) of 3-benzenesulphonyl-5-dimethylaminomethyl-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-7-ol in 50 ml of POCl3 was heated at reflux for 3 hrs. The reaction solution was cooled to RT and evaporated. The residue was treated with 100 ml of ice-water and the pH value of the solution was adjusted to 8 with sat. NaHCO3 solution. The aqueous phase was extracted three times with 100 ml of CH2Cl2 and the organic phases were dried (MgSO4), filtered and evaporated. Chromatography (SiO2, CH2Cl2/AcOEt 1:1) of the residue yielded 1.2 g (88%) of (3-benzenesulphonyl-7-chloro-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-5-ylmethyl)-dimethyl-amine as a colorless foam.

1. temperaturewas heated
2. temperatureat reflux for 3 hrs
3. customevaporated
4. additionThe residue was treated with 100 ml of ice-water
5. extractionThe aqueous phase was extracted three times with 100 ml of CH2Cl2
6. dry with materialthe organic phases were dried (MgSO4)
7. filtrationfiltered
8. customevaporated