Sulfuric acid magnesium salt (1:1) → N-[3-(3-Methoxyphenyl)propylidene]-N'-(4-pyridinyl)hydrazine hydrochloride

HRID 612453

반응식

HRID 612453 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH:11]=O)[CH:6]=[CH:7][CH:8]=1.[ClH:13].[NH:14]([C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1)[NH2:15].S([O-])([O-])(=O)=O.[Mg+2]>C(O)C>[ClH:13].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH:11]=[N:15][NH:14][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[CH:6]=[CH:7][CH:8]=1

참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 114237693-(3-Methoxyphenyl)propionaldehydeHCID 223202584-Hydrazinylpyridine hydrochloride

생성물 1

HCID 70107610N-[3-(3-Methoxyphenyl)propylidene]-N'-(4-pyridinyl)hydrazine hydrochloride수율 61%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A slurry of 3-(3-methoxyphenyl)propionaldehyde (6.46 g), 4-hydrazinopyridine hydrochloride (6.30 g) and magnesium sulfate (5 g) in ethanol (75 ml) was heated under reflux, under nitrogen, with stirring, for 45 mins. The reaction mixture was filtered, the filter cake was washed with ethyl acetate, and the filtrate was concentrated in vacuo. The residue was triturated with ethyl acetate to give 7 g (61%) of product, mp 155-156° C.

후처리

  1. temperatureunder reflux, under nitrogen
  2. filtrationThe reaction mixture was filtered
  3. washthe filter cake was washed with ethyl acetate
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe residue was triturated with ethyl acetate

출처 및 근거

ORD 기록
ord-94ca095354cf45b59cf18d606a9ab0bc
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06004977

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