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Water → HCID 178429062、化合物

HRID 1880689
ノート
印刷プレビュー

反応式

HRID 1880689 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

HCID 178429062HCID 178429062、化合物

実験手順

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)).

後処理

  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

出典と根拠

ORDレコード
ord-1fde040cc6734479ac838e87619a677d
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318776B2

反応ノート

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