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Water → HCID 178429062, 화합물

HRID 1880689
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HRID 1880689 반응식
[O:1]1[CH2:5]CCC1.[CH3:6][C:7]1[N:12]=[C:11]([C:13]([NH2:15])=O)[CH:10]=[C:9]([O:16][CH2:17][C:18]([F:21])([F:20])[F:19])[CH:8]=1.C(N1C=CN=C1)([N:24]1C=CN=C1)=O.N12CCCN=C1CCCCC2.[OH2:45]>>[CH3:6][C:7]1[N:12]=[C:11]([C:13]2[NH:24][O:45][C:5](=[O:1])[N:15]=2)[CH:10]=[C:9]([O:16][CH2:17][C:18]([F:21])([F:20])[F:19])[CH:8]=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 866473336-Methyl-4-(2,2,2-trifluoroethoxy)pyridine-2-carboxamide

생성물 1

HCID 178429062HCID 178429062, 화합물

실험 절차

To 5 ml of tetrahydrofuran were added 0.66 g of 6-methyl-4-(2,2,2-trifluoroethoxy)pyridine-2-carboxamide=oxime and 0.56 g of 1,1′-carbonyldiimidazole, and the mixture was stirred at room temperature for 2 hours. Thereafter, 0.52 g of 1,8-diazabicyclo[5,4,0]undec-7-ene was added at 10° C., and the mixture was stirred for 8 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 0.69 g of 3-[6-methyl-4-(2,2,2-trifluoroethoxy)pyridin-2-yl]-1,2,4-oxadiazol-5-one (present compound (29)).

후처리

  1. stirringthe mixture was stirred for 8 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-1fde040cc6734479ac838e87619a677d
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318776B2

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