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Hydrochloric Acid → [2-(2-Chloro-4-nitro-phenyl)-ethyl]-(4-fluoro-benzyl)-amine hydrochloride

HRID 1019734
ノート
印刷プレビュー

反応式

HRID 1019734 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[CH2:11][CH2:12][NH:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=1.Cl.O1CCOCC1>C(Cl)Cl>[ClH:1].[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[CH2:11][CH2:12][NH:13][CH2:14][C:15]1[CH:16]=[CH:17][C:18]([F:21])=[CH:19][CH:20]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 67465980[2-(2-Chloro-4-nitro-phenyl)-ethyl]-(4-fluoro-benzyl)-amine

生成物 1

HCID 67465979[2-(2-Chloro-4-nitro-phenyl)-ethyl]-(4-fluoro-benzyl)-amine hydrochloride収率 162.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a suspension of [2-(2-chloro-4-nitro-phenyl)-ethyl]-(4-fluoro-benzyl)-amine (3.1 g, 10 mmol) in DCM (31 mL) was added 15% HCl in dioxane (2.4 mL, 10 mmol) at 0° C. and the mixture was maintained for 1 hour at 0° C. After completion of salt formation, the volatiles were removed under reduced pressure. A mixture of 4:1 hexane and ethyl acetate (50 mL) was added to the residue and this was stirred for 15 minutes. The solvent was removed by filtration under suction and the solid was dried under reduced pressure to afford crude title product (2.8 g, 80%).

後処理

  1. customAfter completion of salt formation, the volatiles were removed under reduced pressure
  2. additionA mixture of 4:1 hexane and ethyl acetate (50 mL)
  3. additionwas added to the residue
  4. customThe solvent was removed by filtration under suction
  5. customthe solid was dried under reduced pressure

出典と根拠

ORDレコード
ord-a75c51ec56a947e98b773e94c92821f9
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08716287B2

反応ノート

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