2,4-Dimethoxybenzylamine → N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amine

HRID 537027

反応式

HRID 537027 の反応式
F[C:2]1[CH:7]=[C:6]([I:8])[C:5]([CH3:9])=[CH:4][N:3]=1.[CH3:10][O:11][C:12]1[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:13]=1[CH2:20][NH2:21]>CCOC(C)=O>[CH3:10][O:11][C:12]1[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:13]=1[CH2:20][NH:21][C:2]1[CH:7]=[C:6]([I:8])[C:5]([CH3:9])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 5972502,4-DimethoxybenzylamineHCID 100600522-Fluoro-4-iodo-5-methylpyridine

生成物 1

HCID 66747638N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amine収率 57%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
110 °C

実験手順

A mixture of 2-fluoro-4-iodo-5-methylpyridine (60 g, 253 mmol) and 1-(2,4-dimethoxyphenyl)methanamine (190.6 mL, 1270 mmol) was allowed to stir at 110° C. overnight. The mixture was allowed to cool to rt and was then diluted with EtOAc (190 mL). The resulting solid was filtered and washed with EtOAc and then purified by column chromatography to give N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amine (55.0 g, 57%).

後処理

  1. temperatureto cool to rt
  2. filtrationThe resulting solid was filtered
  3. washwashed with EtOAc
  4. custompurified by column chromatography

出典と根拠

ORDレコード
ord-325d4bda78d84a6fa902d9be0996752d
出典データセット
uspto-grants-2014_10
特許番号
US08859768B2

関連ノート

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