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

HRID 8637

反応式

HRID 8637 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-39687a43224143b2a901aec5623ec2e7
出典データセット
uspto-grants-2006_08
特許番号
US07091199B1

関連ノート

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