Methyl iodide → 2-Methylbenzo(b)thiophene
反応式
[Li][C:2](C)(C)C.[S:6]1[CH:10]=[CH:9][C:8]2[CH:11]=[CH:12][CH:13]=[CH:14][C:7]1=2.C1COCC1.IC>CCOCC>[CH3:2][C:10]1[S:6][C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[CH:9]=1参加物
6
反応条件
- 温度
- -30 °C
実験手順
t-BuLi (1.7M, 26 mmoles, 15 ml) was added to a stirred solution of benzo[b]thiophene (17 mmoles, 2.3 g) and THF (30 ml) at -50° C. The resulting bright yellow reaction mixture was warmed to -30° C., and iodomethane (26 mmoles, 1.6 ml) was added. After 10 min. at -30° C., the solution was warmed to ambient temperature and stirred an additional 30 min., then diluted with ether (100 ml) and washed with brine (2×100 ml). The organic phase was dried (MgSO4), filtered and concentrated to collect 2.48 g (98%) of 2-methylbenzo[b]thiophene as a light yellow solid.
後処理
- temperaturethe solution was warmed to ambient temperature
- washwashed with brine (2×100 ml)
- dry with materialThe organic phase was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customto collect 2.48 g (98%) of 2-methylbenzo[b]thiophene as a light yellow solid
出典と根拠
- ORDレコード
- ord-7907f0755a9a46be993b5afb3b109fd1
- 出典データセット
- uspto-grants-1997_01
- 特許番号
- US05594021
反応ノート
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