Methyl iodide → HCID 22349532, 화합물
반응식
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][CH:8]2[OH:11])=[CH:4][CH:3]=1.[H-].[Na+].I[CH3:15]>O1CCCC1>[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][CH:8]2[O:11][CH3:15])=[CH:4][CH:3]=1참가 물질
5
실험 절차
To a solution of 6-bromoindanol (0.51 g, 2.4 mmol) in anhydrous tetrahydrofuran (10 mL), was added sodium hydride (0.097 g, 3.84 mmol) over a period of five minutes at room temperature. The reaction mixture was stirred at room temperature for fifteen minutes and iodomethane (0.22 mL, 3.6 mmol) was added. After thirty minutes at room temperature, the reaction mixture was partitioned between ethyl acetate (20 mL) and water (20 mL). The ethyl acetate layer was washed with brine (20 mL), dried over sodium sulfate and concentrated to yield the title compound (0.485 g, 89%). 1H NMR (CDCl3) : □ 7.5 (s, 1H), 7.3 (d, 1H), 7.0 (d, 1H), 4.7 (m, 1H), 3.3 (s, 3H), 3.0 (m, 1H), 2.7 (m, 1H), 2.3 (m, 1H), 2.0 (m, 1H).
후처리
- waitAfter thirty minutes at room temperature
- customthe reaction mixture was partitioned between ethyl acetate (20 mL) and water (20 mL)
- washThe ethyl acetate layer was washed with brine (20 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-e819a17da0f845b0bfba26e925c8899f
- 출처 데이터셋
- uspto-grants-2005_07
- 특허 번호
- US06919335B2
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