반응 #657308

반응 방정식

3-phenyl-1H-pyrazol-5-ol

1-bromo-3-chloropropane

potassium carbonate

→

2-phenyl-6,7-dihydro-5H-pyrazolo[5,1-b][1,3]oxazine

용매

acetonitrile

반응 조건

후처리

1. 1
   온도is heated for 5.5 h
2. 2
   온도under reflux
3. 3
   기타Thereafter the volatiles are evaporated
4. 4
   workup.ADDITIONthe residue is treated with 50 mL ethyl acetate
5. 5
   세척The residual solid is washed 2× with ethyl acetate
6. 6
   기타the combined organic phases are evaporated
7. 7
   기타The obtained crude product
8. 8
   기타is triturated with methyl tert butylether and 6.4 g (53%) of 2-phenyl-6,7-dihydro-5H-pyrazolo[5,1-b][1,3]oxazine
9. 9
   기타are obtained as solid

실험 절차

A mixture of 3-phenyl-1H-pyrazol-5-ol (8.80 g, 0.055 mol), 1-bromo-3-chloropropane (9.5 g, 1.1 eq, 0.06 mol) and potassium carbonate (30.3 g, 4 eq, 0.22 mol) in acetonitrile (120 mL) is heated for 5.5 h under reflux. Thereafter the volatiles are evaporated and the residue is treated with 50 mL ethyl acetate. The residual solid is washed 2× with ethyl acetate and the combined organic phases are evaporated. The obtained crude product is triturated with methyl tert butylether and 6.4 g (53%) of 2-phenyl-6,7-dihydro-5H-pyrazolo[5,1-b][1,3]oxazine are obtained as solid.

출처