2-Bromo-1-(3,4-dichlorophenyl)ethanone → HCID 178477975, 화합물

HRID 276771

반응식

HRID 276771 반응식
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

참가 물질

8

반응물 4

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

생성물 1

HCID 178477975HCID 178477975, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6212Chloroform용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-ee9b6e165ef34b6fb9cf15324b2925e1
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355635B1

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