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Water → HCID 178517506, 화합물

HRID 1880664
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HRID 1880664 반응식
[O:1]1[CH2:5]CCC1.[Cl:6][C:7]1[C:8]([C:16]([F:19])([F:18])[F:17])=[CH:9][C:10]([C:13]([NH2:15])=O)=[N:11][CH:12]=1.C(N1C=CN=C1)([N:22]1C=CN=C1)=O.N12CCCN=C1CCCCC2.[OH2:43]>>[Cl:6][C:7]1[C:8]([C:16]([F:19])([F:18])[F:17])=[CH:9][C:10]([C:13]2[NH:22][O:43][C:5](=[O:1])[N:15]=2)=[N:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 962WaterHCID 8028TetrahydrofuranHCID 682631,1'-CarbonyldiimidazoleHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 86647328HCID 86647328, 화합물

생성물 1

HCID 178517506HCID 178517506, 화합물

실험 절차

To 6.6 ml of tetrahydrofuran were added 0.8 g of 5-chloro-4-trifluoromethylpyridine-2-carboxamide=oxime and 0.76 g of 1,1′-carbonyldiimidazole, and the mixture was stirred at room temperature for 1 hour and 30 minutes. Thereafter, 0.71 g of 1,8-diazabicyclo[5,4,0]undec-7-ene was added, and the mixture was stirred for 3 hours. To the reaction solution were added water and a 10% aqueous HCl solution, the resultant solution was extracted with ethyl acetate three times, and the organic layers were combined, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.68 g of 3-(5-chloro-4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-one (present compound (51)).

후처리

  1. stirringthe mixture was stirred for 3 hours
  2. extractiona 10% aqueous HCl solution, the resultant solution was extracted with ethyl acetate three times
  3. dry with materialdried with anhydrous magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f72483ebbd2c461dae6b63ea267685c8
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318776B2

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