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

HRID 276771

反応式

HRID 276771 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 hexamethyldisilazide (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-ee9b6e165ef34b6fb9cf15324b2925e1
出典データセット
uspto-grants-2002_03
特許番号
US06355635B1

関連ノート

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