N-vinyl-2-pyrrolidone → HCID 22037088、化合物

HRID 1864086ノート

反応式

HRID 1864086 の反応式
CO[C:3](=[O:18])[C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[C:6]([C:14]([F:17])([F:16])[F:15])[CH:5]=1.[CH:19]([N:21]1[CH2:25][CH2:24][CH2:23][C:22]1=[O:26])=[CH2:20].[H-].[Na+]>C1(C)C=CC=CC=1>[F:16][C:14]([F:17])([F:15])[C:6]1[CH:5]=[C:4]([CH:9]=[C:8]([C:10]([F:13])([F:11])[F:12])[CH:7]=1)[C:3]([CH:23]1[CH2:24][CH2:25][N:21]([CH:19]=[CH2:20])[C:22]1=[O:26])=[O:18]

参加物

5

反応物 3

HCID 6917N-vinyl-2-pyrrolidoneHCID 24758Sodium hydrideHCID 141265Methyl 3,5-bis(trifluoromethyl)benzoate

生成物 1

HCID 22037088HCID 22037088、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 3,5-bis-(trifluoromethyl)-benzoic acid methyl ester (2 g) and 1-vinyl-2-pyrrolidinone (863 μL) was added to a mixture of sodium hydride (60% suspension in mineral oil-0.41 g) in dry toluene (30 mL) previously heated to reflux. The mixture was stirred for 12 hrs, then it was partitioned between saturated ammonium chloride solution and AcOEt. The organic layer was dried, concentrated in vacuo and the residue was purified by flash chromatography (CH/AcOEt 8:2) to give the title compound (1.6 g) as a beige oil.

後処理

  1. temperaturepreviously heated to reflux
  2. customit was partitioned between saturated ammonium chloride solution and AcOEt
  3. customThe organic layer was dried
  4. concentrationconcentrated in vacuo
  5. customthe residue was purified by flash chromatography (CH/AcOEt 8:2)

出典と根拠

ORDレコード
ord-3434c941d5154236a8ef735b6f09246a
出典データセット
uspto-grants-2009_12
特許番号
US07625904B2

反応ノート

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