Hydrazine hydrate (1:1) → HCID 12297944、化合物

HRID 1730643ノート

反応式

HRID 1730643 の反応式
[NH2:1][C:2]1[N:12]=[C:11]([CH3:13])[C:10]([NH:14][C:15](=[O:17])[CH3:16])=[C:9]([CH3:18])[C:3]=1[C:4](OCC)=[O:5].O.[NH2:20][NH2:21]>O.CO>[NH2:1][C:2]1[N:12]=[C:11]([CH3:13])[C:10]([NH:14][C:15](=[O:17])[CH3:16])=[C:9]([CH3:18])[C:3]=1[C:4]([NH:20][NH2:21])=[O:5]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 12297943HCID 12297943、化合物

生成物 1

HCID 12297944HCID 12297944、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

A mixture of ethyl 2-amino-5-acetamido-4,6-dimethylnicotinate (45.3 g., 0.18 mole) and hydrazine hydrate (100 ml.) is heated in an oil bath with stirring at 120° C. for two hours. The mixture is cooled, the solid collected, and a second crop of solid obtained by evaporating the mother liquor to about half its initial volume. The combined solids melt at 293° C. (dec.), yield 38.1 g. (89%). Analytically pure compound is obtained by dissolving the solid in about six and one-half parts (volume by weight) of hot water and diluting the filtered solution with methanol. The purified product decomposed at about 309° C. with only partial melting.

後処理

  1. temperatureis heated in an oil bath
  2. temperatureThe mixture is cooled
  3. customthe solid collected
  4. customa second crop of solid obtained
  5. customby evaporating the mother liquor to about half its initial volume
  6. customAnalytically pure compound is obtained
  7. customdecomposed at about 309° C. with only partial melting

出典と根拠

ORDレコード
ord-61250c22e6cd452f97f736c68fb8666a
出典データセット
uspto-grants-1976_11
特許番号
US03993656

反応ノート

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