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Methylamine → HCID 10741054, 화합물

HRID 1899096
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HRID 1899096 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][CH:10]=[CH:11][C:12]=2[C:13]2[CH:18]=[CH:17][C:16]([S:19]([CH3:22])(=[O:21])=[O:20])=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.Cl[S:24]([OH:27])(=O)=[O:25].[CH3:28][NH2:29]>O1CCCC1>[CH3:28][NH:29][S:24]([C:10]1[S:9][C:8]([C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=2)=[C:12]([C:13]2[CH:18]=[CH:17][C:16]([S:19]([CH3:22])(=[O:21])=[O:20])=[CH:15][CH:14]=2)[CH:11]=1)(=[O:27])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6329MethylamineHCID 24638Chlorosulfonic acidHCID 103368732-(4-Fluorophenyl)-3-(4-methylsulfonylphenyl)thiophene

생성물 1

HCID 10741054HCID 10741054, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2-(4-Fluorophenyl)-3-[4-(methylsulfonyl)phenyl]thiophene (1.1 g) was added portionwise to chlorosulfonic acid (1 ml), and the mixture was stirred at ambient temperature for 1 hour. The mixture was added to a mixture of 25% methylamine aqueous solution (20 ml) and tetrahydrofuran (20 ml), and stirred at 0° C. for 1 hour. The reaction mixture was extracted with ethyl acetate, and the extract was washed with water, dried and concentrated. The oily residue (2.4 g) was purified by column chromatography on silica gel eluting with a mixture of chloroform and methanol (20:1), and then recrystallized from ethanol to give colorless crystals of N-methyl-5-(4-fluorophenyl)-4-[4-(methylsulfonyl)phenyl]thiophene-2-sulfonamide (1.1 g).

후처리

  1. stirringstirred at 0° C. for 1 hour
  2. extractionThe reaction mixture was extracted with ethyl acetate
  3. washthe extract was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe oily residue (2.4 g) was purified by column chromatography on silica gel eluting with a mixture of chloroform and methanol (20:1)
  7. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-34c7054137cd481cb214312f6f65e969
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05571810

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