Hydrazine hydrate (1:1) → 6-Chloro-3-hydrazinyl-4-methylpyridazine

HRID 873969

반응식

HRID 873969 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[CH3:8].O.[NH2:11][NH2:12]>>[Cl:9][C:5]1[N:4]=[N:3][C:2]([NH:11][NH2:12])=[C:7]([CH3:8])[CH:6]=1

참가 물질

3

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 879233,6-Dichloro-4-methylpyridazine

생성물 1

HCID 114464906-Chloro-3-hydrazinyl-4-methylpyridazine수율 14.8%

반응 조건

온도
80 °C

실험 절차

A mixture of 3,6-dichloro-4-methylpyridazine (5 g, 30.7 mmol) in hydrazine hydrate (30.4 mL, 153 mmol) was heated up and stirred at 80° C. for 24 hr. The reaction was cooled down to RT; the resulting solid was filtrated off, washed with water and dried under reduced pressure. Recrystallization in hot EtOH followed by trituration in EtOH and ultra sounds afforded the title product (721 mg, 4.55 mmol, 14.8% yield) as white solid. tR: 0.34 min (LC-MS 2); ESI-MS: 159 [M+H]+ (LC-MS 2).

후처리

  1. temperaturewas heated up
  2. temperatureThe reaction was cooled down to RT
  3. filtrationthe resulting solid was filtrated off
  4. washwashed with water
  5. customdried under reduced pressure
  6. customRecrystallization in hot EtOH

출처 및 근거

ORD 기록
ord-934d3899d478450293ff5d984e5a67df
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975417B2

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