Ethyl bromoacetate → Ammonia

HRID 20270

反応式

HRID 20270 の反応式
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

参加物

6

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 127492-Methylimidazole

生成物 2

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f852e7f1217c4842882dc23cfb56a9df
出典データセット
uspto-grants-2010_06
特許番号
US07745630B2

関連ノート

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