Dimethylformamide → HCID 57978005、化合物

HRID 1865819ノート

反応式

HRID 1865819 の反応式
[Cl:1][C:2]1[C:3](=[O:10])[NH:4]NC(=O)[C:7]=1[Cl:8].[CH3:11][N:12]([CH:14]=[O:15])C.C(=O)([O-])[O-].[K+].[K+].[CH2:22](Br)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>CCCCCC.O>[CH2:11]([N:12]1[C:14](=[O:15])[C:7]([Cl:8])=[C:2]([Cl:1])[C:3]([O:4][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:10]1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 2414464,5-dichloropyridazine-3,6-diol

生成物 1

HCID 57978005HCID 57978005、化合物収率 90%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8058Hexane溶媒

反応条件

温度
50 °C

実験手順

To a round bottom flask was added 4,5-dichloro-1,2-dihydropyridazine-3,6-dione (20 gm, 73.8 mmol), DMF (200 ml), potassium carbonate (20.36 gm, 147.6 mmol) and benzylbromide (15.14 gm, 88.56 mmol). The reaction was stirred at 50° C. for 6 hrs and then stirred at rt overnight. After this time, the reaction was poured into a 1:1 water: hexane mixture (2000 mL). The resultant mixture was stirred at rt for 1 h. A solid precipitate formed and the precipitate was collected by filtration to give the title compound, 2-benzyl-6-(benzyloxy)-4,5-dichloropyridazin-3(2H)-one (23.9 gm, 90% yield) as light yellow solid. 1(DMSO-D6): 7.45 (m, 2H), 7.35 (m, 4H), 7.30 (m, 4H), 5.26 (s, 2H), 5.17 (s, 2H).

後処理

  1. stirringstirred at rt overnight
  2. customA solid precipitate formed
  3. filtrationthe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-4ce057238e3e4cd8b8988856ab745695
出典データセット
uspto-grants-2009_12
特許番号
US07629342B2

反応ノート

読み込み中…