Ethyl bromoacetate → Ammonia

HRID 20270

반응식

HRID 20270 반응식
C(=O)([O-])[O-].[K+].[K+].[CH3:7][C:8]1[NH:9][CH:10]=[CH:11][N:12]=1.Br[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]>O1CCCC1>[NH3:9].[CH3:7][C:8]1[N:9]([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH:10]=[CH:11][N:12]=1

참가 물질

6

반응물 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 127492-Methylimidazole

생성물 2

HCID 222AmmoniaHCID 28940035Ethyl (2-methyl-1H-imidazol-1-yl)acetate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Potassium carbonate (8.42 g, 61 mmol) was added to a solution of 2-methylimidazole (5 g, 61 mmol) in tetrahydrofuran (100 mL) and the suspension was stirred for 30 minutes. Ethyl bromoacetate (6.75 mL, 61 mmol) was added and the reaction was stirred for a further 30 minutes at room temperature. The mixture was filtered, washing through with dichloromethane:methanol (90:10). The filtrate was evaporated under reduced pressure and the crude product was purified by column chromatography on silica gel using dichloromethane:methanol:0.88 ammonia (93:7:0.5) as eluant to afford the title compound as an oil, 5.28 g.

후처리

  1. stirringthe reaction was stirred for a further 30 minutes at room temperature
  2. filtrationThe mixture was filtered
  3. washwashing through with dichloromethane:methanol (90:10)
  4. customThe filtrate was evaporated under reduced pressure
  5. customthe crude product was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-f852e7f1217c4842882dc23cfb56a9df
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745630B2

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