Hydrazine → HCID 58772592、化合物

HRID 2250352ノート

反応式

HRID 2250352 の反応式
[NH2:1][NH2:2].[Cl:3][C:4]1[N:5]=[N:6][C:7](Cl)=[CH:8][C:9]=1[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=1>N1C=CC=CC=1>[Cl:3][C:4]1[N:5]=[N:6][C:7]([NH:1][NH2:2])=[CH:8][C:9]=1[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=1

参加物

4

反応物 2

HCID 9321HydrazineHCID 58772591HCID 58772591、化合物

生成物 1

HCID 58772592HCID 58772592、化合物収率 57%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
100 °C

実験手順

Anhydrous hydrazine (8 mL) was added to a solution of 3,6-dichloro-4-(4-chlorophenyl)pyridazine (7.1 g, 27.4 mmol) in pyridine (30 mL) at 100° C. The resulting mixture was stirred at 100° C. for 30 min. Analysis by HPLC/MS indicated the reaction was complete. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure to remove most of the pyridine. To the residue was added isopropanol (200 mL), the resulting suspension was refluxed for 20 min. After cooling to room temperature, the suspension was filtered. The collected solid was washed with isopropanol, dried in a 50° C. vacuum oven overnight to afford 4.0 g (57%) of the title compound as an off-white solid. LC/MS (method A): retention time=2.24 min, (M+H)+=255.

後処理

  1. temperatureAfter cooling to room temperature
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customto remove most of the pyridine
  4. additionTo the residue was added isopropanol (200 mL)
  5. temperaturethe resulting suspension was refluxed for 20 min
  6. temperatureAfter cooling to room temperature
  7. filtrationthe suspension was filtered
  8. washThe collected solid was washed with isopropanol
  9. customdried in a 50° C. vacuum oven overnight

出典と根拠

ORDレコード
ord-2920fb589f9441aca1570fa6d3f0c11a
出典データセット
uspto-grants-2008_01
特許番号
US07317012B2

反応ノート

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