Dichloromethane → 2-Amino-3-(2,4,6-trifluorobenzyloxy)pyridine

HRID 1654910

反応式

HRID 1654910 の反応式
[NH2:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.ClCCl.[OH-].[Na+].[F:14][C:15]1[CH:22]=[C:21]([F:23])[CH:20]=[C:19]([F:24])[C:16]=1[CH2:17]Br>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].O>[NH2:1][C:2]1[C:7]([O:8][CH2:17][C:16]2[C:15]([F:14])=[CH:22][C:21]([F:23])=[CH:20][C:19]=2[F:24])=[CH:6][CH:5]=[CH:4][N:3]=1

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 281142-Amino-3-HydroxypyridineHCID 27770592,4,6-Trifluorobenzyl bromide

生成物 1

HCID 100151612-Amino-3-(2,4,6-trifluorobenzyloxy)pyridine

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 pyridine (2.44 g, 0.022 mol), dichloromethane (20 ml) and 40% aqueous sodium hydroxide solution (20 ml) was stirred for five minutes, then 2,4,6-trifluorobenzyl bromide (5.00 g, 0.022 mol) and Adogen 464 (3 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 ether gave the desired product. Yield 2.76 g (49%), m.p. 122°-124 ° 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 ether

出典と根拠

ORDレコード
ord-bb33cbd7b8a34d758b52d28e57911d25
出典データセット
uspto-grants-1995_04
特許番号
US05409943

関連ノート

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