Dimethyl Sulfate → 3,5-diamino-1-methyl-1H-pyrazole-4-carbonitrile

HRID 261073ノート

反応式

HRID 261073 の反応式
[NH2:1][C:2]1[C:6]([C:7]#[N:8])=[C:5]([NH2:9])[NH:4][N:3]=1.[CH3:10]OS(OC)(=O)=O>[OH-].[Na+]>[NH2:1][C:2]1[C:6]([C:7]#[N:8])=[C:5]([NH2:9])[N:4]([CH3:10])[N:3]=1

参加物

4

反応物 2

HCID 6497Dimethyl SulfateHCID 142021413,5-Diamino-1H-pyrazole-4-carbonitrile

生成物 1

HCID 126210283,5-diamino-1-methyl-1H-pyrazole-4-carbonitrile収率 20.8%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

3,5-Diamino-4-cyanopyrazole (6.1 g) was dissolved in 1 M sodium hydroxide solution (50 ml), and dimethylsulphate (6.2 g) was added. The mixture was heated at reflux for 21/2 hours and then evaporated to dryness. The residue was extracted with 2-methoxyethanol, and the extracts were evaporated. The residue was triturated with a small amount of water to give 3,5-diamino-4-cyano-1-methylpyrazole (1.4 g), m.p. 194°-196° C.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 21/2 hours
  3. customevaporated to dryness
  4. extractionThe residue was extracted with 2-methoxyethanol
  5. customthe extracts were evaporated
  6. customThe residue was triturated with a small amount of water

出典と根拠

ORDレコード
ord-d64a01b7bcd6409887b9085dfe54487f
出典データセット
uspto-grants-1979_08
特許番号
US04163846

反応ノート

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