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Methyl 2,2,2-trichloroacetimidate → 6-fluoro-1-(4-methoxybutyl)-2-(trichloromethyl)-1H-benzimidazole

HRID 1259911
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HRID 1259911 반응식
[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([NH:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH3:15])[CH:3]=1.[Cl:16][C:17]([Cl:23])([Cl:22])[C:18](=N)OC>C(O)(=O)C>[F:1][C:2]1[CH:8]=[CH:7][C:5]2[N:6]=[C:18]([C:17]([Cl:23])([Cl:22])[Cl:16])[N:9]([CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH3:15])[C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 100479Methyl 2,2,2-trichloroacetimidateHCID 583555474-Fluoro-2-(4-methoxybutylamino)aniline

생성물 1

HCID 583553976-fluoro-1-(4-methoxybutyl)-2-(trichloromethyl)-1H-benzimidazole

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

4-Fluoro-2-(4-methoxybutylamino)aniline (4.28 g) was dissolved in acetic acid (100 ml), methyl 2,2,2-trichloroethanimidate (2.49 ml) was added dropwise, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, and the residue was azeotroped with toluene. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate was concentrated under reduced pressure to give the object product (6.53 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was azeotroped with toluene
  3. washa fraction eluted with ethyl acetate
  4. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-83f1d3f08eae456e99540787c04071f0
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08466282B2

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