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Hydroxyamine hydrochloride → HCID 178526352, 화합물

HRID 897998
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반응식

HRID 897998 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])=S)=[CH:4][CH:3]=1.Cl.[NH2:19][OH:20].C(=O)(O)[O-].[Na+]>C(O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[N:19][OH:20])[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 22346994HCID 22346994, 화합물

생성물 1

HCID 178526352HCID 178526352, 화합물수율 77.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of N1-(4-bromophenyl)-2-fluoro-1-benzenecarbothioamide (1.56 g, 0.00505 mol), hydroxylamine hydrochloride (0.44 g, 0.00631 mol) and sodium bicarbonate (0.53 g, 0.00631 mol) was heated in absolute ethanol (25 mL) at reflux under nitrogen atmosphere for 14 hours. The reaction mixture was cooled to ambient temperature, the solvent was removed under reduced pressure and the residue partitioned between saturated solution of sodium bicarbonate in water (50 mL) and ethyl acetate (50 mL). The organic phase was washed with brine, dried with magnesium sulfate and concentrated. The residue was suspended in cold diethyl ether and the precipitate was collected by filtration and dried to yield N1-(4-bromophenyl)-2-fluoro-1-benzeneamidoxime (1.21 g, 0.00392 mol) as an off-white solid.

후처리

  1. temperatureat reflux under nitrogen atmosphere for 14 hours
  2. customthe solvent was removed under reduced pressure
  3. customthe residue partitioned between saturated solution of sodium bicarbonate in water (50 mL) and ethyl acetate (50 mL)
  4. washThe organic phase was washed with brine
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated
  7. filtrationthe precipitate was collected by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-9644a091f2c84cba85ac83fe665f356e
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06921763B2

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