Hydrochloric Acid → HCID 178517505、化合物

HRID 1880663ノート

反応式

HRID 1880663 の反応式
[F:1][C:2]1[N:7]=[C:6]([C:8]([NH2:10])=O)[CH:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[CH:3]=1.[C:15](N1C=CN=C1)(N1C=CN=C1)=[O:16].[N:27]12CCCN=C1CCCCC2.Cl.[OH2:39]>O1CCCC1>[F:1][C:2]1[N:7]=[C:6]([C:8]2[NH:27][O:39][C:15](=[O:16])[N:10]=2)[CH:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[CH:3]=1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 962WaterHCID 682631,1'-CarbonyldiimidazoleHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 86647327HCID 86647327、化合物

生成物 1

HCID 178517505HCID 178517505、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 5 ml of tetrahydrofuran were added 0.6 g of 6-fluoro-4-trifluoromethylpyridine-2-carboxamide=oxime and 0.61 g of 1,1′-carbonyldiimidazole, and the mixture was stirred at room temperature for 2 hours and 30 minutes. Thereafter, 0.57 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 10% HCl, the resultant solution was extracted with ethyl acetate three times, and the organic layers were combinedmm, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.5 g of 3-(6-fluoro-4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-one (present compound (49)).

後処理

  1. stirringthe mixture was stirred for 9 hours
  2. extractionthe 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-0ceb2f76703644adb05d0a392fe379b7
出典データセット
uspto-grants-2012_11
特許番号
US08318776B2

反応ノート

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