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

HRID 873973노트

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HRID 873973 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 2500056-Chloro-3-hydrazinylpyridazin-4-amine수율 33%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-fe5ad3ee10bd4892b72eb56e37fdebf1
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975417B2

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