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Methanol → N[2-(Bromoacetyl-phenyl)-1,1-dimethyl-ethyl]-2,2,2-trifluoroacetamide

HRID 413297
ノート
印刷プレビュー

反応式

HRID 413297 の反応式
[CH3:1][C:2]([NH:11][C:12](=[O:17])[C:13]([F:16])([F:15])[F:14])([CH3:10])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Br-:18].[Br-].[Br-].C([N+](CC[CH2:36][CH3:37])(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C[OH:73]>C(Cl)Cl>[Br:18][CH2:36][C:37]([C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[CH2:3][C:2]([NH:11][C:12](=[O:17])[C:13]([F:16])([F:14])[F:15])([CH3:1])[CH3:10])=[O:73]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 592937N-(1,1-Dimethyl-2-phenylethyl)-2,2,2-trifluoroacetamideHCID 23500184Tetra-n-butylammonium tribromide

生成物 1

HCID 18523616N[2-(Bromoacetyl-phenyl)-1,1-dimethyl-ethyl]-2,2,2-trifluoroacetamide収率 41%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a round-bottomed flask, N-(1,1-dimethyl-2-phenyl-ethyl)-2,2,2-trifluoroacetamide (6.90 g, 21.0 mmol) was dissolved in methylene chloride (66 ml) and methanol (33 ml). Tetrabutylammonium tribromide (10.6 g, 22.0 mmol) was added to this solution in one portion, and the mixture was allowed to stir at room temperature overnight. The volatiles were then removed in vacuo to an oil, which was then resuspended in 100 ml of methylene chloride and extracted with 125 ml of saturated aqueous sodium bicarbonate. The aqueous extracts were reextracted with methylene chloride (3×10 ml), and the combined organic extracts were then washed with water and dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude oil was purified by column chromatography (silica gel; 60% methylene chloride/hexanes to 10% ethyl acetate/methylene chloride), and the resulting material (5.18 g) was recrystallized from hexanes to afford 3.14 g (41% yield) of pure product as a fluffy white solid.

後処理

  1. customThe volatiles were then removed in vacuo to an oil, which
  2. extractionextracted with 125 ml of saturated aqueous sodium bicarbonate
  3. washthe combined organic extracts were then washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude oil was purified by column chromatography (silica gel; 60% methylene chloride/hexanes to 10% ethyl acetate/methylene chloride)
  8. customthe resulting material (5.18 g) was recrystallized from hexanes

出典と根拠

ORDレコード
ord-41063e03b7694b15a21a98ceb95a9117
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06566377B2

反応ノート

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