Allyl bromide → 3-(allyloxy)-N,N-dimethylpropan-1-amine

HRID 58002

반응식

HRID 58002 반응식
[H-].[Na+].[CH3:3][N:4]([CH3:9])[CH2:5][CH2:6][CH2:7][OH:8].[CH2:10](Br)[CH:11]=[CH2:12]>CC(C)=O>[CH2:12]([O:8][CH2:7][CH2:6][CH2:5][N:4]([CH3:9])[CH3:3])[CH:11]=[CH2:10]

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 24758Sodium hydrideHCID 766463-(Dimethylamino)-1-propanol

생성물 1

HCID 226500083-(allyloxy)-N,N-dimethylpropan-1-amine

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
0 °C

실험 절차

Sodium hydride (17.5 g) and dimethyl formaldehyde (400 mL) were added to a 2-L round-bottom flask. After cooling the flask to 0° C. by immersing in an ice bath, 3-dimethylamino-1-propanol (0.398 mol) was added. After stirring for about 30 minutes and adding allyl bromide (0.4378 mol), the mixture was stirred for 3 hours after raising the temperature of the reactor to room temperature. Upon completion of reaction, the reaction was terminated by adding water to the flask and the product was extracted using diethyl ether. The extract was concentrated under reduced pressure and used in the next step without further purification. After filtration under reduced pressure, 3-(allyloxy)-N,N-dimethylpropan-1-amine was obtained through fractional distillation. Structural analysis was performed by NMR spectroscopy.

후처리

  1. customby immersing in an ice bath
  2. stirringthe mixture was stirred for 3 hours
  3. temperatureafter raising the temperature of the reactor to room temperature
  4. customUpon completion of reaction
  5. customthe reaction was terminated
  6. additionby adding water to the flask
  7. extractionthe product was extracted
  8. concentrationThe extract was concentrated under reduced pressure
  9. customused in the next step without further purification
  10. filtrationAfter filtration under reduced pressure

출처 및 근거

ORD 기록
ord-18e2561901ff49ad83a89a70e1d2ff11
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434751B2

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