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Hydroxyamine hydrochloride → HCID 73516783, 화합물

HRID 482149
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반응식

HRID 482149 반응식
[F:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:8]=[C:9]([C:13]3[CH2:17][CH2:16][C:15](=O)[CH:14]=3)[CH:10]=[CH:11][CH:12]=2)=[CH:4][CH:3]=1.Cl.[NH2:22][OH:23]>>[F:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:8]=[C:9]([C:13]3[CH2:17][CH2:16][C:15](=[N:22][OH:23])[CH:14]=3)[CH:10]=[CH:11][CH:12]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 19065571HCID 19065571, 화합물

생성물 1

HCID 73516783HCID 73516783, 화합물수율 113.6%

실험 절차

To a stirred solution of 3-[3-(4-fluorophenoxy)phenyl]-2-cyclopentenone (10 g; 0.0373M) in ethanol-pyridine (75 ml-21 ml) was added hydroxylamine hydrochloride (3.37 g; 0.0485M) at room temperature. After stirring for 4 hrs, solvent was removed. To the residue was added dilute aqueous HCl (100 ml), and the whole was extracted with ethyl acetate (200 ml×1, 100 ml×1). The combined organic layers were washed with water (100 ml), brine (100 ml), dried over MgSO4, and concentrated in vacuo to give 12 g of crude subtitle compound [E] as a brown oil, which was used without further purification.

후처리

  1. customsolvent was removed
  2. additionTo the residue was added dilute aqueous HCl (100 ml)
  3. extractionthe whole was extracted with ethyl acetate (200 ml×1, 100 ml×1)
  • washThe combined organic layers were washed with water (100 ml), brine (100 ml)
  • dry with materialdried over MgSO4
  • concentrationconcentrated in vacuo
  • 출처 및 근거

    ORD 기록
    ord-83e7addb87c64214b6be58776e2478cc
    출처 데이터셋
    uspto-grants-1998_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05792882

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