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HCID 18956529, 화합물 → 2-(2,4-Difluorophenyl)-3-(pyridin-2-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol

HRID 2380036
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HRID 2380036 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1([CH:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=2)[CH3:13])[CH2:11][O:10]1.[Na].[NH:21]1[CH:25]=[N:24][CH:23]=[N:22]1>CN(C)C=O>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:10])([CH:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1)[CH3:13])[CH2:11][N:21]1[CH:25]=[N:24][CH:23]=[N:22]1
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참가 물질

4

반응물 2

HCID 18956529HCID 18956529, 화합물HCID 454898221h-1,2,4-Triazole sodium salt

생성물 1

HCID 193659342-(2,4-Difluorophenyl)-3-(pyridin-2-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of the product of part (i) (2.20 g) and 1H-1,2,4-triazole sodium salt (1.53 g) in N,N-dimethylformamide (15 ml) was heated at 60° with stirring for 18 hours and then evaporated. Water (50 ml) was added and the mixture was extracted with ethyl acetate (3×50 ml). The combined extracts were dried (Na2SO4), evaporated and the residue was chromatographed on silica gel. Elution with ethyl acetate first gave, after combination and evaporation of appropriate fractions, the title compound, diastereoisomeric pair A, (0.93 g), m.p. 146°-148° (from ether).

후처리

  1. temperaturewas heated at 60°
  2. customevaporated
  3. additionWater (50 ml) was added
  4. extractionthe mixture was extracted with ethyl acetate (3×50 ml)
  5. dry with materialThe combined extracts were dried (Na2SO4)
  6. customevaporated
  7. customthe residue was chromatographed on silica gel
  8. washElution with ethyl acetate
  9. customfirst gave
  10. customafter combination and evaporation of appropriate fractions

출처 및 근거

ORD 기록
ord-57e96e6fc1814a7f8aec7a9917f0379f
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05364938

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