t-Butyl bromide → 5-Tert-butylthiophene-2-carboxylic acid
반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([OH:8])=[O:7].[C:9](Br)([CH3:12])([CH3:11])[CH3:10]>C(Cl)Cl>[CH3:10][C:9]([C:5]1[S:1][C:2]([C:6]([OH:8])=[O:7])=[CH:3][CH:4]=1)([CH3:12])[CH3:11]참가 물질
4
실험 절차
To a solution of 5.0 g (39.02 mmol) of thiophene-2-carboxylic acid (Aldrich Chemical Co.) in 100 mL of methylene chloride stirred at 0° C. was added 11 g (82.5 mmol) of AICl3 and 5.8 g (43.0 mmol) of t-butyl bromide. The solution was stirred at room temperature for 18 hours then poured into 100 mL of ice water, and the mixture was extracted with ether. The extracts were washed with brine and dried over MgSO4, then concentrated to give 3.33 g of the title product. MS (M+H)+ : 202. NMR (CDCl3) δ:1.42 (s, 9H), 6.89 (d, 1H, J=4 Hz), 7.72 (d, 1H, J=4 Hz).
후처리
- extractionthe mixture was extracted with ether
- washThe extracts were washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-50183175bd994b62ad3037b69ae3b2c7
- 출처 데이터셋
- uspto-grants-1997_01
- 특허 번호
- US05597832
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