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Benzyl Bromide → HCID 19088497、化合物

HRID 1463290
ノート
印刷プレビュー

反応式

HRID 1463290 の反応式
[CH3:1][C:2]([NH:10][CH3:11])([CH3:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH2:12](Br)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:12]([N:10]([C:2]([CH3:1])([CH3:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH3:11])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 19088476Ethyl 3-methyl-3-(methylamino)butanoate

生成物 1

HCID 19088497HCID 19088497、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture containing ethyl 3-methyl-3-methylaminobutanoate (95 g--Preparation 5), benzyl bromide (72 ml), anhydrous potassium carbonate (138 g) and acetonitrile (500 ml) was heated under reflux for 1.5 hours. The mixture was concentrated in vacuo and the residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml). The layers were separated and the aqueous layer extracted with dichloromethane (2 ×100 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give an the title compound as a mobile, colourless oil, yield, 150 g.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1.5 hours
  3. concentrationThe mixture was concentrated in vacuo
  4. customthe residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml)
  5. customThe layers were separated
  6. extractionthe aqueous layer extracted with dichloromethane (2 ×100 ml)
  7. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5a422e6d4926448c830c5282e0e9fa30
出典データセット
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05300516

反応ノート

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