Ammonium Hydroxide → 3,5-Dichloro-1,4-dihydropyridazin-4-imine

HRID 1845998노트

반응식

HRID 1845998 반응식
[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([Cl:9])[C:7]=1Cl.[NH4+:10].[OH-]>CCO>[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([Cl:9])[C:7]=1[NH2:10]

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 701113,4,5-Trichloropyridazine

생성물 1

HCID 64032013,5-Dichloro-1,4-dihydropyridazin-4-imine수율 36%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
120 °C

실험 절차

A mixture of 3,4,5-trichloropyridazine (Preparation 3, 500 mg, 2.73 mmole) in EtOH (5.5 mL) and NH4OH (5.5 mL) was heated under microwave irradiation 120° C. for 25 minutes. Concentration under reduced pressure and purification via silica gel column chromatography eluting with acetone:dichloromethane (0-15% acetone), provided the title product in 36% yield, 163 mg.

후처리

  1. concentrationConcentration
  2. customunder reduced pressure and purification via silica gel column chromatography
  3. washeluting with acetone

출처 및 근거

ORD 기록
ord-684ad457d66744869237a591806839a4
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952008B2

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