Hydrazine hydrate (1:1) → 6-Chloro-3-hydrazinylpyridazin-4-amine

HRID 873973ノート

反応式

HRID 873973 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[NH2:8].O.[NH2:11][NH2:12]>CCO>[Cl:9][C:5]1[N:4]=[N:3][C:2]([NH:11][NH2:12])=[C:7]([NH2:8])[CH:6]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 2984983,6-Dichloropyridazin-4-amine

生成物 1

HCID 2500056-Chloro-3-hydrazinylpyridazin-4-amine収率 33%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

To a stirred suspension of 3,6-dichloropyridazin-4-amine (Step 112.1) (1.49 g, 9.09 mmol) in EtOH (15 mL) was added hydrazine hydrate (11.04 mL, 227 mmol) and the resulting mixture was heated up and stirred at 100° C. for 3 hr. The reaction was cooled down to RT and concentrated under reduced pressure. The crude product was triturated with water (25 mL) to afford the title product (478 mg, 3 mmol, 33% yield) as yellow solid. tR: 0.24 min (LC-MS 2); ESI-MS: 160 [M+H]+ (LC-MS 2); ESI-MS: 158 [M−H]− (LC-MS 2).

後処理

  1. temperaturethe resulting mixture was heated up
  2. temperatureThe reaction was cooled down to RT
  3. concentrationconcentrated under reduced pressure
  4. customThe crude product was triturated with water (25 mL)

出典と根拠

ORDレコード
ord-fe5ad3ee10bd4892b72eb56e37fdebf1
出典データセット
uspto-grants-2015_03
特許番号
US08975417B2

反応ノート

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