Trifluoroacetic acid → Ethyl[4-(1,1-dimethyl-2-{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}ethyl)-2-methylphenoxy]acetate

HRID 9691

反応式

HRID 9691 の反応式
[CH2:1]([O:3][C:4](=[O:35])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:33])([CH3:32])[C:14]([C:16]2[S:17][C:18]([C:22]3[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=3)=[CH:19][C:20]=2[CH3:21])=O)=[CH:9][C:8]=1[CH3:34])[CH3:2].FC(F)(F)C(O)=O.C([SiH](CC)CC)C>>[CH2:1]([O:3][C:4](=[O:35])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:32])([CH3:33])[CH2:14][C:16]2[S:17][C:18]([C:22]3[CH:23]=[CH:24][C:25]([C:28]([F:29])([F:30])[F:31])=[CH:26][CH:27]=3)=[CH:19][C:20]=2[CH3:21])=[CH:9][C:8]=1[CH3:34])[CH3:2]

参加物

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 21986375Ethyl[4-(1,1-dimethyl-2{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}-2-oxoethyl)-2-methylphenoxy]acetate2 回

生成物 1

HCID 21986315Ethyl[4-(1,1-dimethyl-2-{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}ethyl)-2-methylphenoxy]acetate

反応条件

温度
50 °C

実験手順

To a reactivial containing ethyl[4-(1,1-dimethyl-2-{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}-2-oxoethyl)-2-methylphenoxy]acetate (intermediate 106, 36 mg) was added trifluoroacetic acid (0.22 ml) and triethylsilane (0.11 ml). The vial was then sealed and heated at 50° C. for 18 hours. The reaction was then allowed to cool to room and concentrated in vacuo. Purification by flash column chromatography eluting cyclohexane-1% EtOAc/cyclohexane yielded the title compound as a colourless oil.

後処理

  1. customThe vial was then sealed
  2. temperatureto cool to room
  3. concentrationconcentrated in vacuo
  4. customPurification by flash column chromatography
  5. washeluting cyclohexane-1% EtOAc/cyclohexane

出典と根拠

ORDレコード
ord-91be913968d14eb2aa60244378ae719c
出典データセット
uspto-grants-2006_08
特許番号
US07091237B2

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