Hydrazine hydrate (1:1) → 5-Cyano-2-hydrazino-4-methylamino-pyrimidine

HRID 1586404ノート

反応式

HRID 1586404 の反応式
[C:1]([C:3]1[C:4]([NH:11][CH3:12])=[N:5][C:6](SC)=[N:7][CH:8]=1)#[N:2].O.[NH2:14][NH2:15]>C(O)C>[C:1]([C:3]1[C:4]([NH:11][CH3:12])=[N:5][C:6]([NH:14][NH2:15])=[N:7][CH:8]=1)#[N:2]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 106789344-(Methylamino)-2-(methylthio)pyrimidine-5-carbonitrile

生成物 1

HCID 218527585-Cyano-2-hydrazino-4-methylamino-pyrimidine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 5-cyano-4-methylamino-2-methylsulfanyl-pyrimidine (25.86 g) from Example 3 and hydrazine hydrate (52 mL) in ethanol (250 mL) was heated at reflux with stirring for 3 hours. The reaction mixture was cooled to room temperature and the insoluble product was collected by filtration, washed with cold aqueous ethanol (1:1) to give 23 g of the title compound. Crystallization from ethanol afforded an analytically pure sample of 5-cyano-2-hydrazino-4-methylamino-pyrimidine; mp 247-249° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux
  3. filtrationthe insoluble product was collected by filtration
  4. washwashed with cold aqueous ethanol (1:1)

出典と根拠

ORDレコード
ord-ed3f60ed5811407d9d82a3513081be99
出典データセット
uspto-grants-1999_08
特許番号
US05945422

反応ノート

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