2-Bromo-1-(3,4-dichlorophenyl)ethanone → HCID 178477975、化合物

HRID 1057304ノート

反応式

HRID 1057304 の反応式
C[Si](C)(C)[N-:3][Si](C)(C)C.[Li+].[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]#[N:19])=[CH:14][N:13]=1.C(=O)(O)[O-].[Na+].[Cl:25][C:26]1[CH:27]=[C:28]([CH:33]=[CH:34][C:35]=1[Cl:36])[C:29](=O)[CH2:30]Br>C1COCC1.C(Cl)(Cl)Cl.O>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[NH:3][CH:30]=[C:29]([C:28]3[CH:33]=[CH:34][C:35]([Cl:36])=[C:26]([Cl:25])[CH:27]=3)[N:19]=2)=[CH:14][N:13]=1

参加物

8

反応物 4

HCID 2447512-Bromo-1-(3,4-dichlorophenyl)ethanoneHCID 516892Sodium BicarbonateHCID 2733832Lithium HexamethyldisilazideHCID 51520946-Chloro-3-pyridinecarbonitrile

生成物 1

HCID 178477975HCID 178477975、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6212Chloroform溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Lithium hexamethyidisilazide (41.5 mL of a 1.0 M solution in THF) was added to a solution of 2-chloro-5-cyanopyridine (5.24 g) in THF (10 mL). The resultant mixture was stirred at room temperature for 30 min, and then 13 mL saturated aqueous sodium bicarbonate and 5 mL water were added to the reaction mixture. A solution of 3,4-dichlorophenacyl bromide (10.13 g) in chloroform (150 mL) was added in two portions approximately 15 min apart. The resultant mixture was stirred for 72 hours, and the reaction mixture was filtered. The filter cake was triturated with dichloromethane (50 mL) to provide 2-Chloro-5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridine (10.46 g). MS m/z 324 (M+), 326 (M++2).

後処理

  1. filtrationthe reaction mixture was filtered
  2. customThe filter cake was triturated with dichloromethane (50 mL)

出典と根拠

ORDレコード
ord-e4aa31441ee94d3197a4b2b527c19426
出典データセット
uspto-grants-2003_02
特許番号
US06514966B2

反応ノート

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