Water → 4,4-Dimethyl-1-n-butyl-2-undecyl-2-imidazoline

HRID 1086446

반응식

HRID 1086446 반응식
[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].[CH3:6][C:7]1([CH3:23])[CH2:11][NH:10][C:9]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])=[N:8]1.BrCCCC.O>CCCCCC.C1C=CC=CC=1>[CH3:6][C:7]1([CH3:23])[CH2:11][N:10]([CH2:1][CH2:2][CH2:3][CH3:4])[C:9]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])=[N:8]1

참가 물질

7

반응물 4

HCID 962WaterHCID 8002Butyl bromideHCID 178418339ButyllithiumHCID 1784428094,4-Dimethyl-2-undecyl-2-imidazoline

생성물 1

HCID 146517984,4-Dimethyl-1-n-butyl-2-undecyl-2-imidazoline수율 67%

시약·촉매·용매 2

HCID 241Benzene용매HCID 8058Hexane용매

실험 절차

22 ml (55 mmoles) of a 2.5M solution of butyl lithium in hexane are added to 12.62 g (50 mmoles) of 4,4-dimethyl-2-undecyl-2-imidazoline in 50 ml of anhydrous benzene at a temperature kept at around 20° C. The mixture is then stirred for 2 hours at ambient temperature (15° to 20° C.). 8.22 g (60 mmoles) of 1-bromobutane is then added dropwise to the reaction mixture, keeping the temperature at around 20° C. The reaction mixture is then stirred at ambient temperature until it is homogenous, after which it is refluxed for 3 hours. After cooling, 50 ml of water is added, the mixture is stirred for half hour, decanted and extracted with 100 ml of ether. After drying over magnesium sulfate the solvent is removed in vacuo and the oil is distilled at reduced pressure to give 10.34 g (67%) of the product.

후처리

  1. customkept at around 20° C
  2. customat around 20° C
  3. stirringThe reaction mixture is then stirred at ambient temperature until it
  4. temperatureafter which it is refluxed for 3 hours
  5. temperatureAfter cooling
  6. stirringthe mixture is stirred for half hour
  7. customdecanted
  8. extractionextracted with 100 ml of ether
  9. dry with materialAfter drying over magnesium sulfate the solvent
  10. customis removed in vacuo
  11. distillationthe oil is distilled at reduced pressure

출처 및 근거

ORD 기록
ord-1946623e2769422a83a8f9c1e2c41239
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05030629

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