2-(2,4-Difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol → Hydrogen Bromide

HRID 1654230노트

반응식

HRID 1654230 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@:9]([OH:19])([C@H:16]([SH:18])[CH3:17])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.[BrH:20].C(O)(=O)C>C(OCC)(=O)C.CCCCCC>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@:9]([OH:19])([C@H:16]([SH:18])[CH3:17])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.[BrH:20]

참가 물질

6

반응물 2

HCID 1922642-(2,4-Difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol2회HCID 21893785Acetic Acid Mixture with Hydrobromic Acid

생성물 2

HCID 260Hydrogen BromideHCID 1922642-(2,4-Difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol

시약·촉매·용매 2

HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

In ethyl acetate (20 ml) was dissolved (2R,3R)-2-(2,4-difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol (compound 43, 0.48 g) followed by addition of 25% hydrogen bromide-acetic acid (0.7 ml). The reaction mixture was diluted with 100 ml of hexane and the resulting powder was collected by filtration and dissolved in ethyl acetate (10 ml). The solution was allowed to stand after addition of ethyl ether (20 ml) and the resulting crystals were collected by filtration to yield compound 43 hydrobromide (0.35 g) as colorless platelets. m.p. 180°-185° C.

후처리

  1. filtrationthe resulting powder was collected by filtration
  2. dissolutiondissolved in ethyl acetate (10 ml)
  3. additionafter addition of ethyl ether (20 ml)
  4. filtrationthe resulting crystals were collected by filtration

출처 및 근거

ORD 기록
ord-bfc9862910f14fc68ca5d93888f7035d
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05405861

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