6-Amino-3-chloropyridazine → 6-(4-Benzylpiperazin-1-yl)pyridazin-3-ylamine

HRID 80717

反応式

HRID 80717 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:14][C:15]1[N:16]=[N:17][C:18](Cl)=[CH:19][CH:20]=1>C(=O)(O)[O-].[Na+]>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:18]2[N:17]=[N:16][C:15]([NH2:14])=[CH:20][CH:19]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 216436-Amino-3-chloropyridazineHCID 759941-Benzylpiperazine

生成物 1

HCID 593677126-(4-Benzylpiperazin-1-yl)pyridazin-3-ylamine収率 82.2%

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

実験手順

48.9 g (278 mmol) of 1-benzylpiperazine and 12.0 g (92.6 mmol) of 3-amino-6-chloropyridazine are heated at 160° C. for 1 hour. The brown oil obtained is poured into 500 mL of aqueous sodium bicarbonate solution and the product is extracted with dichloromethane. The organic phase is dried and then concentrated under reduced pressure. The oil obtained is triturated in diethyl ether, and 20.5 g of a solid are isolated after filtering off and drying.

後処理

  1. customThe brown oil obtained
  2. extractionthe product is extracted with dichloromethane
  3. customThe organic phase is dried
  4. concentrationconcentrated under reduced pressure
  5. customThe oil obtained
  6. customis triturated in diethyl ether

出典と根拠

ORDレコード
ord-365f660cdcd04b8c95be9d01d77f0cb0
出典データセット
uspto-grants-2014_09
特許番号
US08846676B2

関連ノート

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