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

HRID 612453

反応式

HRID 612453 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94ca095354cf45b59cf18d606a9ab0bc
出典データセット
uspto-grants-1999_12
特許番号
US06004977

関連ノート

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