p-Toluenesulfonic acid → 1H-Indene, 2-methyl-
반응식
[CH3:1][C:2]1(O)[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>CCCCCC>[CH3:1][C:2]1[CH2:10][C:9]2[C:4]([CH:3]=1)=[CH:5][CH:6]=[CH:7][CH:8]=2참가 물질
4
실험 절차
25.5 g (0.17 moles) of compound 12, 3.2 g (0.017 moles) of p-toluenesulfonic acid and 500 ml of hexane were placed in a round-bottomed flask fitted with a Dean-Stark apparatus. This suspension was refluxed for 3 h. After cooling, the hexane fraction was decanted from the insoluble products and the solvent was removed under vacuum to leave an oil, which was then distilled in a short distillation column at 45° C. and 0.03 mbar to give 15 g (yield: 68%) of compound 13. 1H NMR (400 MHz, CDCl3): δ=7.33 (d, J=7.6 Hz. 1H); 7.21 (m, 2H); 7.06 pseudo dt, J=7.2, 1.4 Hz, 1H); 6.45 (bs, 1H); 3.25 (s, 2H); 2.12 (s, 3H).
후처리
- customfitted with a Dean-Stark apparatus
- temperatureThis suspension was refluxed for 3 h
- temperatureAfter cooling
- customthe hexane fraction was decanted from the insoluble products
- customthe solvent was removed under vacuum
- customto leave an oil, which
- distillationwas then distilled in a short distillation column at 45° C.
출처 및 근거
- ORD 기록
- ord-b470cb38e86c46dfbfed47983cb39ff2
- 출처 데이터셋
- uspto-grants-2002_08
- 특허 번호
- US06433112B1
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