6-Amino-3-chloropyridazine → HCID 178484245、化合物

HRID 2176619

反応式

HRID 2176619 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][CH:3]=1.CO[CH:11](OC)[N:12]([CH3:14])[CH3:13]>>[Cl:1][C:2]1[N:7]=[N:6][C:5](/[N:8]=[CH:11]/[N:12]([CH3:14])[CH3:13])=[CH:4][CH:3]=1

参加物

3

反応物 2

HCID 216436-Amino-3-chloropyridazineHCID 78373Dimethylformamide dimethyl acetal

生成物 1

HCID 178484245HCID 178484245、化合物収率 82.9%

反応条件

温度
110 °C

実験手順

A 500 mL RB flask was charged with 6-chloropyridazin-3-amine (10.0 g, 77.2 mmol) and dimethoxy-N,N-dimethylmethanamine (206 ml, 1544 mmol), equipped with a reflux condenser, then heated to 110° C. for 3 hours then left at room temperature for 16 hours. The precipitate was collected by filtration. The mother liquor was concentrated down to give an yellow solid, which was triturated with EtOAc and collected. The solids were combined to give (E)-N′-(6-chloropyridazin-3-yl)-N,N-dimethylformamidine (11.81 g, 82.9% yield) as a white solid

後処理

  1. customequipped with a reflux condenser
  2. filtrationThe precipitate was collected by filtration
  3. concentrationThe mother liquor was concentrated down
  4. customto give an yellow solid, which
  5. customwas triturated with EtOAc
  6. customcollected

出典と根拠

ORDレコード
ord-866037ccb2c548d89a4cadf36b178b9f
出典データセット
uspto-grants-2015_06
特許番号
US09066954B2

関連ノート

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