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

HRID 1845998ノート

反応式

HRID 1845998 の反応式
[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]

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 701113,4,5-Trichloropyridazine

生成物 1

HCID 64032013,5-Dichloro-1,4-dihydropyridazin-4-imine収率 36%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-684ad457d66744869237a591806839a4
出典データセット
uspto-grants-2015_02
特許番号
US08952008B2

反応ノート

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