t-Butyl bromide → 5-Tert-butylthiophene-2-carboxylic acid
反応式
[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]参加物
4
実験手順
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).
後処理
- extractionthe mixture was extracted with ether
- washThe extracts were washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-50183175bd994b62ad3037b69ae3b2c7
- 出典データセット
- uspto-grants-1997_01
- 特許番号
- US05597832
反応ノート
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