Hydroxyamine hydrochloride → Trifluoromethyl(3,4-methylenedioxyphenyl)methanone-oxime

HRID 580546노트

반응식

HRID 580546 반응식
[F:1][C:2]([C:5]([C:7]1[CH:12]=[CH:11][C:10]2[O:13][CH2:14][O:15][C:9]=2[CH:8]=1)=O)([F:4])[F:3].Cl.[NH2:17][OH:18].C([O-])(=O)C.[Na+]>CO.O>[F:1][C:2]([C:5]([C:7]1[CH:12]=[CH:11][C:10]2[O:13][CH2:14][O:15][C:9]=2[CH:8]=1)=[N:17][OH:18])([F:4])[F:3]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 108464551-(1,3-Benzodioxol-5-YL)-2,2,2-trifluoro-ethanone

생성물 1

HCID 72726727Trifluoromethyl(3,4-methylenedioxyphenyl)methanone-oxime수율 76.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

Trifluoromethyl(3,4-methylenedioxyphenyl) methanone (1.46 g, 0.0067 mole), hydroxylamine hydrochloride (1.06 g), 0.015 mole) and sodium acetate (0.86 g, 0.010 mole) were dissolved in a mixture of methanol (4 ml) and water (4 ml) and heated to reflux for 4.5 hours. After cooling to room temperature, water (10 ml) was added and the mixture extracted with ether (3×15 ml). The combined extracts were washed with water (20 ml) and brine (20 ml) and dried over anhydrous sodium sulfate. After filtration and removal of the solvent in vacuo the residue was recrystallized from a mixture of dichloromethane and petroleum spirit (40°-60° C.) to give trifluoromethyl(3,4-methylenedioxyphenyl)methanone-oxime (1.2 g), (76.9%) m.p. 96.0° C.

후처리

  1. temperatureheated
  2. temperatureto reflux for 4.5 hours
  3. extractionthe mixture extracted with ether (3×15 ml)
  4. washThe combined extracts were washed with water (20 ml) and brine (20 ml)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationAfter filtration and removal of the solvent in vacuo the residue
  7. customwas recrystallized from a mixture of dichloromethane and petroleum spirit (40°-60° C.)

출처 및 근거

ORD 기록
ord-c3624a3e22724cd0909943c201dae39e
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04753960

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