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Trifluoroacetic acid → 3-(4-Imidazol-1-ylmethylphenyl)-5-butylthiophene-2-sulfonamide

HRID 1993840
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HRID 1993840 반응식
FC(F)(F)C(O)=O.[N:8]1([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:24]=[C:23]([CH2:25][CH2:26][CH2:27][CH3:28])[S:22][C:21]=3[S:29]([NH:32]C(C)(C)C)(=[O:31])=[O:30])=[CH:16][CH:15]=2)[CH:12]=[CH:11][N:10]=[CH:9]1.BrC1C=CC(CN2C=CN=C2)=CC=1>C1(OC)C=CC=CC=1>[N:8]1([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:24]=[C:23]([CH2:25][CH2:26][CH2:27][CH3:28])[S:22][C:21]=3[S:29]([NH2:32])(=[O:31])=[O:30])=[CH:16][CH:15]=2)[CH:12]=[CH:11][N:10]=[CH:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 29895571-(4-Bromobenzyl)-1H-imidazoleHCID 119940313-(4-Imidazol-1-ylmethylphenyl)-5-butyl-N-tert-butylthiophene-2-sulfonamide

생성물 1

HCID 667751023-(4-Imidazol-1-ylmethylphenyl)-5-butylthiophene-2-sulfonamide수율 49%

시약·촉매·용매 1

HCID 7519Anisole촉매

실험 절차

Trifluoroacetic acid was added (10 mL) to the crude 3-(4-imidazol-1-ylmethylphenyl)-5-butyl-N-tert-butylthiophene-2-sulfonamide from step (c) above, and one drop (ca. 0.05 mL) of anisol was added to the mixture. The reaction mixture was stirred under N2 atmosphere for 30 hours and then evaporated and co-evaporated with acetonitrile. The crude product was purified by column chromatography (CH2Cl2:MeOH (20:1)) to give sub-title compound (232 mg, 0.62 mmol) in 49% yield (from 1-(4-bromobenzyl)-1H-imidazole).

후처리

  1. additionwas added to the mixture
  2. customevaporated
  3. customThe crude product was purified by column chromatography (CH2Cl2:MeOH (20:1))

출처 및 근거

ORD 기록
ord-4ec81581c941495c8643a85ff2afee5d
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652054B2

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