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

HRID 873969

反応式

HRID 873969 の反応式
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

参加物

3

反応物 2

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

生成物 1

HCID 114464906-Chloro-3-hydrazinyl-4-methylpyridazine収率 14.8%

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-934d3899d478450293ff5d984e5a67df
出典データセット
uspto-grants-2015_03
特許番号
US08975417B2

関連ノート

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