Dichloromethane → HCID 20076964、化合物

HRID 1654916ノート

反応式

HRID 1654916 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]([O:23][CH3:24])[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:21]([O:23][CH3:24])=[CH:22][C:15]=2[F:14])=[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 109550331-(Bromomethyl)-2-fluoro-4-methoxybenzene

生成物 1

HCID 20076964HCID 20076964、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 (1.45g, 0.013 mol), dichloromethane (10 ml) and 40% aqueous sodium hydroxide solution (10 ml) was stirred for five minutes, then 2-fluoro-4-methoxybenzyl bromide (2.9 g, 0.013 mol) and Adogen 464 (1.5 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 ether gave the desired product. Yield 1.11 g (34%), m.p. 135°-138 ° 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-b05def9f119c48999a142c4a4225eb8e
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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