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

HRID 1531820

反応式

HRID 1531820 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-2de880554d7644f69b61d9ba078c0f35
出典データセット
uspto-grants-2001_03
特許番号
US06200982B1

関連ノート

読み込み中…