N-Methylbenzylamine → 4-(N-benzyl-N-methylaminoacetyl)pyridine

HRID 275763

反応式

HRID 275763 の反応式
[CH2:1]([NH:8][CH3:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br.Br[CH2:12][C:13]([C:15]1[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=1)=[O:14]>ClCCl>[CH2:1]([N:8]([CH2:12][C:13]([C:15]1[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=1)=[O:14])[CH3:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 7669N-MethylbenzylamineHCID 27762394-(Bromoacetyl)pyridine hydrobromide

生成物 1

HCID 700736314-(N-benzyl-N-methylaminoacetyl)pyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of N-benzyl-N-methylamine (3.7 cm3) in dry dichloromethane (40 cm3), cooled to 0° C. was added with stirring, 4-bromoacetylpyridine hydrobromide (4.0 g). The reaction was allowed to warm to room temperature, then stirred for a further 18 hr. The solvent was stripped at reduced pressure, and the residue partitioned between ethyl acetate and dilute aqueous Na2CO3. The organic phase was separated, dried (Na2SO4), evaporated, and the residue subjected to chromatography on silica gel, eluent 5% methanol in dichloromethane, to afford 4-(N-benzyl-N-methylaminoacetyl)pyridine, 1.49 g, 43%, as a yellow gum.

後処理

  1. additionwas added
  2. stirringstirred for a further 18 hr
  3. customthe residue partitioned between ethyl acetate and dilute aqueous Na2CO3
  4. customThe organic phase was separated
  5. dry with materialdried (Na2SO4)
  6. customevaporated

出典と根拠

ORDレコード
ord-699ebe2269e54c3fa8fd56c24fea2b67
出典データセット
uspto-grants-2002_03
特許番号
US06352994B2

関連ノート

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