O-Xylene → 4-Propylpyridin-2-amine

HRID 487999

反応式

HRID 487999 の反応式
[CH2:1]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)[CH2:2][CH3:3].[NH2-:10].[Na+].C1(C)C(C)=CC=CC=1>O>[NH2:10][C:6]1[CH:5]=[C:4]([CH2:1][CH2:2][CH3:3])[CH:9]=[CH:8][N:7]=1

参加物

5

反応物 3

HCID 7237O-XyleneHCID 24533Sodium amide2 回HCID 707384-Propylpyridine

生成物 1

HCID 70225944-Propylpyridin-2-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

75 g (0.62M) of 4-n-propylpyridine and 28 g (0.73M) of sodium amide were added to 250 ml of xylene, and the mixture was heated under reflux for 10 hr. Water was added in small portions to the reaction mixture under ice cooling to decompose excess sodium amide, and the reaction mixture was extracted with ethyl acetate, dried over magnesium sulfate and then purified by column chromatography (dichloromethanemethanol 50:1→20:1). The yield was 33 g. (blackish purple solid)

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 10 hr
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. dry with materialdried over magnesium sulfate
  5. custompurified by column chromatography (dichloromethanemethanol 50:1→20:1)

出典と根拠

ORDレコード
ord-99275caca2504d5a8f8480478f041851
出典データセット
uspto-grants-1994_03
特許番号
US05298518

関連ノート

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