N-vinyl-2-pyrrolidone → HCID 22037088, 화합물

HRID 1864086노트

반응식

HRID 1864086 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 22037088HCID 22037088, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-3434c941d5154236a8ef735b6f09246a
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625904B2

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