反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[O:13][CH:12]=[C:11]([CH2:14]O)[CH:10]=2)=[CH:5][CH:4]=1.C(P(CCCC)CCCC)CCC.[CH2:31]([O:33][C:34](=[O:45])[CH2:35][O:36][C:37]1[CH:42]=[CH:41][C:40]([SH:43])=[CH:39][C:38]=1[CH3:44])[CH3:32]>O1CCCC1>[CH2:31]([O:33][C:34](=[O:45])[CH2:35][O:36][C:37]1[CH:42]=[CH:41][C:40]([S:43][CH2:14][C:11]2[CH:10]=[C:9]([C:6]3[CH:7]=[CH:8][C:3]([C:2]([F:17])([F:16])[F:1])=[CH:4][CH:5]=3)[O:13][CH:12]=2)=[CH:39][C:38]=1[CH3:44])[CH3:32]参加物
5
実験手順
A solution of {5-[4-(trifluoromethyl)phenyl]-3-furyl}methanol (0.15 g) in tetrahydrofuran (15 ml) stirred at 0° C. was treated with tributylphosphine (0.2 ml), as solution of ethyl(4-mercapto-2-methylphenoxy)acetate (0.150 g) in tetrahydrofuran (2 ml) and finally azodicarbonyldimorpholide (0.204 g). The reaction was allowed to warm to ambient temperature and stirred for 18 hours. The solvent was evaporated and the residue subjected to an aqueous work up using ethyl acetate and water. The organic phase was dried over magnesium sulfate. The product isolated after evaporation of the solvent was further purified by flash column chromatography using a cyclohexane:ethyl acetate (5:1) as eluent to give the title compound.
後処理
- customThe solvent was evaporated
- dry with materialThe organic phase was dried over magnesium sulfate
- customThe product isolated
- customafter evaporation of the solvent
- customwas further purified by flash column chromatography
出典と根拠
- ORDレコード
- ord-e19001d0595c45359652e9e2aef71108
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091237B2
関連ノート
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