Dichloromethane → HCID 12758273、化合物

HRID 1654884ノート

反応式

HRID 1654884 の反応式
[NH2:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.Cl[CH2:10][Cl:11].[OH-].[Na+].Cl[C:15]1[CH:22]=C[CH:20]=[CH:19][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[CH:19]=[CH:20][C:10]([Cl:11])=[CH:22][CH:15]=2)=[CH:6][CH:5]=[CH:4][N:3]=1

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 11905alpha-Bromo-o-chlorotolueneHCID 14798Sodium HydroxideHCID 281142-Amino-3-Hydroxypyridine

生成物 1

HCID 12758273HCID 12758273、化合物

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 (3.45 g, 0.313 mol), dichloromethane (20 ml) and 40% aqueous sodium hydroxide solution (20 ml) was stirred for five minutes, then 2chlorobenzyl bromide (6.09 g, 0.0315 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 3.5 g (48%), m.p. 121°-123 ° 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-23eb50db7f2b45cd92f413edf74688d1
出典データセット
uspto-grants-1995_04
特許番号
US05409943

反応ノート

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