Sodium → (3-Fluoro-benzyl)-[2-(3-thieno[2,3-d]isoxazol-3-yl-phenoxy)-ethyl]-amine

HRID 8637

반응식

HRID 8637 반응식
[Na].[O:2]1[C:6]2[CH:7]=[CH:8][S:9][C:5]=2[C:4]([C:10]2[CH:11]=[C:12]([OH:16])[CH:13]=[CH:14][CH:15]=2)=[N:3]1.Br[CH2:18][CH2:19][NH:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[CH:23]=1>C1(C)C=CC=CC=1>[F:28][C:24]1[CH:23]=[C:22]([CH:27]=[CH:26][CH:25]=1)[CH2:21][NH:20][CH2:19][CH2:18][O:16][C:12]1[CH:13]=[CH:14][CH:15]=[C:10]([C:4]2[C:5]3[S:9][CH:8]=[CH:7][C:6]=3[O:2][N:3]=2)[CH:11]=1

참가 물질

5

반응물 3

HCID 5360545SodiumHCID 140972423-Thieno[2,3-d]isoxazol-3-yl-phenolHCID 21983578(2-Bromo-ethyl)-(3-fluorobenzyl)-amine

생성물 1

HCID 9907296(3-Fluoro-benzyl)-[2-(3-thieno[2,3-d]isoxazol-3-yl-phenoxy)-ethyl]-amine

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Add dichloromethane to 3-thieno[2,3-d]isoxazol-3-yl-phenol (10 g, 0.046 mol) or the appropriately protected 3-thieno[2,3-d]isoxazol-3-yl-phenol as is known in the art, and stir with sodium hydroxide (1M; 28 mL) to form the sodium salt. Combine the sodium salt from 3-thieno[2,3-d]isoxazol-3-yl-phenol, (2-bromo-ethyl)-(3-fluorobenzyl)-amine (37.5 g, 0.161 mol) in toluene (100 mL) and heat (reflux) for 24 hours. Allow to cool, filter the reaction mixture and evaporate off the solvent to give the final, desired compound. Compound may be purified by distillation under reduced pressure.

후처리

  1. temperatureheat
  2. temperature(reflux) for 24 hours
  3. temperatureAllow to cool
  4. filtrationfilter the reaction mixture
  5. customevaporate off the solvent

출처 및 근거

ORD 기록
ord-39687a43224143b2a901aec5623ec2e7
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091199B1

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