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Water → HCID 178517508、化合物

HRID 1880665
ノート
印刷プレビュー

反応式

HRID 1880665 の反応式
[O:1]1[CH2:5]CCC1.[F: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]>>[F: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
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 86647329HCID 86647329、化合物

生成物 1

HCID 178517508HCID 178517508、化合物

実験手順

To 4 ml of tetrahydrofuran were added 0.4 g of 5-fluoro-4-trifluoromethylpyridine-2-carboxamide=oxime and 0.41 g of 1,1′-carbonyldiimidazole, and the mixture was stirred at room temperature for 2 hours. Thereafter, 0.38 g of 1,8-diazabicyclo[5,4,0]undec-7-ene was added, and the mixture was stirred for 9 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 0.35 g of 3-(5-fluoro-4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-one (present compound (52)).

後処理

  1. stirringthe mixture was stirred for 9 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-2caff9738e6c46778d35a75b64b41c32
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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