Methylamine → 2-(Methylamino)quinolin-8-ol

HRID 493333ノート

反応式

HRID 493333 の反応式
Cl[C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[C:5]([OH:12])[CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH2:13][CH3:14]>CCO>[CH3:14][NH:13][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[C:5]([OH:12])[CH:6]=[CH:7][CH:8]=2)[N:3]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 2748782-Chloroquinolin-8-ol

生成物 1

HCID 13808762-(Methylamino)quinolin-8-ol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

To a solution of 2-chloro-8-hydroxyquinoline* (2.0 g, 11. I mmol) in EtOH (40 mL) was added H2NMe (40% aqueous solution, 40 mL, 464 mmol). The mixture was heated in a sealed Pyrex tube at 100° C. for 24 h. The solvent was evaporated and the resulting crude product was purified by column chromatography [gradient: CH2Cl2/MeOH (99:1) to 1% NH4OH in CH2Cl2/MeOH (80 20)] to give the title compound as a black-green solid Yield 1 31 g (67%), MS m/z 174 (M)+. Anal. (C10H10N2O) C, H, N

後処理

  1. customThe solvent was evaporated
  2. customthe resulting crude product was purified by column chromatography [gradient: CH2Cl2/MeOH (99:1) to 1% NH4OH in CH2Cl2/MeOH (80 20)]

出典と根拠

ORDレコード
ord-e3d7154dc74b42578604ae75c4777b5a
出典データセット
uspto-grants-2009_05
特許番号
US07534794B2

反応ノート

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