Dichloromethane → 2-Amino-3-(2-chloro-6-fluorobenzyloxy)-6-methylpyridine

HRID 1654930

反応式

HRID 1654930 の反応式
[NH2:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1.ClCCl.[OH-].[Na+].[Cl:15][C:16]1[CH:23]=[CH:22][CH:21]=[C:20]([F:24])[C:17]=1[CH2:18]Cl>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].O>[NH2:1][C:2]1[C:7]([O:8][CH2:18][C:17]2[C:20]([F:24])=[CH:21][CH:22]=[CH:23][C:16]=2[Cl:15])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 885002-Amino-6-methylpyridin-3-olHCID 1086751-Chloro-2-(chloromethyl)-3-fluorobenzene

生成物 1

HCID 200769742-Amino-3-(2-chloro-6-fluorobenzyloxy)-6-methylpyridine

試薬・触媒・溶媒 2

HCID 21218Trioctylmethylammonium chloride触媒HCID 962Water溶媒

実験手順

A mixture of 2-amino-3-hydroxy-6-methylpyridine (4.3 g, 0.035 mol), dichloromethane (26 ml) and 40% aqueous sodium hydroxide solution (26 ml) was stirred for five minutes at room temperature, then 2-chloro-6-fluorobenzyl chloride (6.8 g, 0.038 mol) and Adogen 464 (2.5 ml) were added and stirring continued for 16 hours. The mixture was diluted with water and extracted with dichloromethane. Drying and evaporation of the organic extracts and trituration with ethanol gave the desired product. Yield 6.3 g (67%), m.p. 108°-109 ° C.

後処理

  1. stirringstirring
  2. waitcontinued for 16 hours
  3. extractionextracted with dichloromethane
  4. customDrying
  5. customevaporation of the organic extracts and trituration with ethanol

出典と根拠

ORDレコード
ord-c73661605cef49ffab5025d851406823
出典データセット
uspto-grants-1995_04
特許番号
US05409943

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