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

HRID 1019734
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HRID 1019734 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-a75c51ec56a947e98b773e94c92821f9
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716287B2

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