반응 #1687632

반응 방정식

charcoal

acetone oxime

nicotinoyl chloride

ether

→

82

4-Methyl-2-(3-pyridyl)-oxazole

용매

ammonia

—

ice water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise under a nitrogen atmosphere
2. 2
   기타A violent reaction
3. 3
   온도After cooling the mixture
4. 4
   여과filtered
5. 5
   기타the ether phase separated
6. 6
   추출The aqueous phase was extracted with 2×200 ml of ether
7. 7
   건조the combined organic phase dried over magnesium sulphate
8. 8
   기타Removal of solvent in vacuo

실험 절차

To 10 g (0.140 mol) of acetone oxime cooled to -10° C. neat nicotinoyl chloride (40 g, 0.280 mol) was added dropwise under a nitrogen atmosphere. A violent reaction occured and the mixture became quickly solid. The solid was heated to 120° C. for 3 h. After cooling the mixture was dissolved in ice water and ammonia. After addition of 300 ml of ether the mixture was treated with charcoal, filtered, and the ether phase separated. The aqueous phase was extracted with 2×200 ml of ether, and the combined organic phase dried over magnesium sulphate. Removal of solvent in vacuo gave crude 82 as a red oil. Yield: 3.9 g (0.024 mol, 17%).

출처