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

HRID 9691

반응식

HRID 9691 반응식
[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]

참가 물질

4

반응물 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 21986375Ethyl[4-(1,1-dimethyl-2{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}-2-oxoethyl)-2-methylphenoxy]acetate2회

생성물 1

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

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-91be913968d14eb2aa60244378ae719c
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091237B2

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