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m-Chloroperbenzoic acid → HCID 18956544, 화합물

HRID 2380057
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HRID 2380057 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:24])([CH:16]([C:18]1[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=1)[CH3:17])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.ClC1C=C(C=CC=1)C(OO)=[O:30]>ClCCl>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:24])([CH:16]([C:18]1[CH:19]=[CH:20][N+:21]([O-:30])=[CH:22][CH:23]=1)[CH3:17])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1
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반응물 2

HCID 70297m-Chloroperbenzoic acid2회HCID 189565112-(2,4-Difluorophenyl)-3-(pyridin-4-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol

생성물 1

HCID 18956544HCID 18956544, 화합물수율 95.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2-(2,4-difluorophenyl)-3-(pyridin-4-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol (diastereoisomeric pair B from Example 2) (20.0 g) and 85% w/w 3-chloroperoxybenzoic acid (12.3 g) in dichloromethane (250 ml) was stirred at room temperature for 18 hours. Further 3-chloroperoxybenzoic acid (2.50 g) was then added and stirring was continued for 24 hours. The solution was evaporated and the residue was dissolved in ether. A solid formed on standing which was filtered off and chromatographed on silica gel. Elution with dichloromethane/methanol/0.88 ammonia solution (100:4:0.5) gave the title compound as a solid, (20.0 g), m.p. 195°-198°.

후처리

  1. customThe solution was evaporated
  2. dissolutionthe residue was dissolved in ether
  3. customA solid formed on standing which
  4. filtrationwas filtered off
  5. customchromatographed on silica gel
  6. washElution with dichloromethane/methanol/0.88 ammonia solution (100:4:0.5)

출처 및 근거

ORD 기록
ord-29440b86d937456c9de92c858e5510d7
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05364938

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