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

HRID 275763

반응식

HRID 275763 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-699ebe2269e54c3fa8fd56c24fea2b67
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06352994B2

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