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

HRID 1654910
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HRID 1654910 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 21218Trioctylmethylammonium chloride촉매
HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-bb33cbd7b8a34d758b52d28e57911d25
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05409943

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