Hydrazine hydrate (1:1) → HCID 12297944, 화합물

HRID 1730643노트

반응식

HRID 1730643 반응식
[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]

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 12297943HCID 12297943, 화합물

생성물 1

HCID 12297944HCID 12297944, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-61250c22e6cd452f97f736c68fb8666a
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03993656

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