Anthranilic Acid → 1,4-Ethanonaphthalene, 1,4-dihydro-
반응식
[C:1](O)(=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)N.[CH:11]1[CH2:16]CC=[CH:13][CH:12]=1.N(O[CH2:20]CC(C)C)=O>O1CCCC1>[CH:2]12[CH2:8][CH2:7][CH:6]([C:5]3[C:3]1=[CH:13][CH:12]=[CH:11][CH:16]=3)[CH:20]=[CH:1]2참가 물질
5
실험 절차
A THF solution of 1 g (7.3 mmol) of anthranilic acid was dropped into a mixed solution under reflux of 0.77 ml (8.0 mmol) of 1,3-cyclohexadiene, 1.1 ml of isoamyl nitrite and 50 ml of tetrahydrofuran. Then, the resultant solution was heated and refluxed for 2 hours to remove THF, extracted with chloroform, washed with distilled water and saturated saline, dried with anhydrous sodium sulfate and purified with silica gel column-chromatography-(chloroform) to obtain 1,4-dihydro-1,4-ethanonaphthalene (0.89 g, 5.7 mmol, yield: 78%).
후처리
- temperaturerefluxed for 2 hours
- customto remove THF
- extractionextracted with chloroform
- washwashed with distilled water and saturated saline
- dry with materialdried with anhydrous sodium sulfate
- custompurified with silica gel column-chromatography-(chloroform)
출처 및 근거
- ORD 기록
- ord-a17440283c1b4d1dba9b75e78b2c71b4
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07094625B2
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