3-Methyl-8-methylidene-2,4,5,7,8,8a-hexahydroazulen-6(1H)-one → 1,4-Dimethyl-6-oxo-2,3,3a,4,5,6,7,8-octahydroazulene
반응식
[CH3:1][C:2]1[CH2:3][CH2:4][CH:5]2[C:11]=1[CH2:10][CH2:9][C:8](=[O:12])[CH2:7][C:6]2=[CH2:13].[H][H]>C(O)(=O)C.C=C>[CH3:1][C:2]1[CH2:3][CH2:4][CH:5]2[C:11]=1[CH2:10][CH2:9][C:8](=[O:12])[CH2:7][CH:6]2[CH3:13]참가 물질
4
실험 절차
528 mg of 1-methyl-4 -methylen-6-oxo-2,3,3a,4,5,6,7,8-octahydroazulene were hydrogenated in 20 ml of ethylene acetate with the aid of 200 mg of palladium-on-calcium carbonate (5%). After hydrogen uptake was completed the mixture was filtered off from the catalyst, the filtrate concentrated under reduced pressure and distilled. There was obtained pure 1,4-dimethyl-6-oxo-2,3,3a,4,5,6,7,8-octahydroazulene, b.p.0.06 60°; IR(film):νmax = 1700, 1450, 1378, 1250, 1190 cm-1. The compound was a woody, earthy, camphorous odour.
후처리
- filtrationwas filtered off from the catalyst
- concentrationthe filtrate concentrated under reduced pressure
- distillationdistilled
출처 및 근거
- ORD 기록
- ord-9fe8d923c2444d6494d51378ce6521ab
- 출처 데이터셋
- uspto-grants-1977_05
- 특허 번호
- US04024188
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