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Dimethylamine → Dimethyl(3-(3-pyridyloxy)propyl)amine

HRID 2305697
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HRID 2305697 반응식
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1.[CH3:12][NH:13][CH3:14]>CO>[CH3:12][N:13]([CH3:14])[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 184333433-(3-Chloro-propoxy)-pyridine

생성물 1

HCID 9794053Dimethyl(3-(3-pyridyloxy)propyl)amine수율 92.9%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
100 °C

실험 절차

The 3-chloro-1-(3-pyridyloxy)propane (2.00 g, 11.65 mmol) was dissolved in methanol (25 mL) and added to a 40 wt % aqueous solution of dimethylamine (50 mL) in a heavy-walled glass pressure-tube apparatus. The tube was sealed and the mixture was stirred and heated at 100° C. (oil bath temperature) for 4 h. After cooling, the mixture was concentrated by rotary evaporation. Saturated NaCl solution (25 mL) was added to the residue. The pH of the solution was adjusted to 6, and the mixture was extracted with ether (3×25 mL) to remove impurities. The aqueous layer was basified to pH 10 with 10% NaOH solution and extracted with chloroform (4×50 mL). The combined chloroform extracts were dried (Na2SO4), filtered, and concentrated to give 1.95 g (92.9%) of an oil.

후처리

  1. customThe tube was sealed
  2. temperatureAfter cooling
  3. concentrationthe mixture was concentrated by rotary evaporation
  4. additionSaturated NaCl solution (25 mL) was added to the residue
  5. extractionthe mixture was extracted with ether (3×25 mL)
  6. customto remove impurities
  7. extractionextracted with chloroform (4×50 mL)
  8. dry with materialThe combined chloroform extracts were dried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0c8a300fc684477c9bfaed0c76cb5716
출처 데이터셋
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06441006B2

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