反应详情

温度

0 °C

A mixture of 3-(1H-pyrazol-1-yl)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine (I107)(14.3 mg, 0.075 mmol) and triethylamine (0.016 ml, 0.113 mmol) was stirred in Dichloromethane (DCM) (1 ml) at 0° C. and 2,4-dichloro-3-fluorobenzoyl chloride (18.81 mg, 0.083 mmol) in DCM (0.5 ml) was added and the mixture was stirred at 0° C. After 1 h, sat. NaHCO3 (1 ml) and ethyl acetate (30 ml) were added and the product was extracted into ethyl acetate. The organic layer was dried (Na2SO4) and evaporated. Chromatography (SP4 50-100% ethyl acetate in isohexane) gave a crude product which was passed through an SCX column (elution with 2M NH3 in MeOH) to give clean desired product as a gum. This was triturated with ether/hexane to give a white solid in 22.4 mg.

1. extractionthe product was extracted into ethyl acetate
2. dry with materialThe organic layer was dried (Na2SO4)
3. customevaporated
4. customChromatography (SP4 50-100% ethyl acetate in isohexane) gave a crude product which
5. washwas passed through an SCX column (elution with 2M NH3 in MeOH)