Hydrazine → HCID 58772592, 화합물

HRID 2250352노트

반응식

HRID 2250352 반응식
[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

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 58772591HCID 58772591, 화합물

생성물 1

HCID 58772592HCID 58772592, 화합물수율 57%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2920fb589f9441aca1570fa6d3f0c11a
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07317012B2

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