Sodium hydride → 8-fluoro-3,4-dihydro-2H-1,5-benzoxathiepine
反応式
[H-].[Na+].F[C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[S:11][CH2:12][CH2:13][CH2:14][OH:15]>CN(C=O)C>[F:10][C:8]1[CH:7]=[CH:6][C:5]2[S:11][CH2:12][CH2:13][CH2:14][O:15][C:4]=2[CH:9]=1参加物
4
実験手順
Sodium hydride (60% dispersion in mineral oil) (177 mg, 4.42 mmol) was added to a solution of 3-[(2,4-difluorophenyl)thio]propan-1-ol (0.41 g, 2.01 mmol) in DMF (40 mL) and the mixture stirred at RT for 24 hours. The solvent was removed in vacuo and iced water (200 mL) added. The mixture was extracted into ethyl acetate and the organics washed with brine (40 mL), dried (MgSO4), filtered and reduced in vacuo to give a white solid which was chromatographed on silica, eluting with 0-10% ethyl acetate in isohexane, to give the desired compound as a colourless oil (110 mg).
後処理
- customThe solvent was removed in vacuo and iced water (200 mL)
- additionadded
- extractionThe mixture was extracted into ethyl acetate
- washthe organics washed with brine (40 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customto give a white solid which
- customwas chromatographed on silica
- washeluting with 0-10% ethyl acetate in isohexane
出典と根拠
- ORDレコード
- ord-bb2f8f483ed64533a82b93a0a91eecd2
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07943607B2
反応ノート
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