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

HRID 1654930

반응식

HRID 1654930 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 21218Trioctylmethylammonium chloride촉매HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c73661605cef49ffab5025d851406823
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05409943

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