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Chloroform → HCID 21409913, 화합물

HRID 1283547
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HRID 1283547 반응식
[ClH:1].Cl.[CH3:3][N:4]([CH3:10])[C:5]([CH3:9])([CH3:8])[CH2:6][NH2:7].[OH-].[Na+].[CH:13](Cl)(Cl)[Cl:14].[H-].[Al+3].[Li+].[H-].[H-].[H-]>O.CCOCC>[ClH:14].[ClH:1].[CH3:13][NH:7][CH2:6][C:5]([N:4]([CH3:10])[CH3:3])([CH3:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6212ChloroformHCID 14798Sodium HydroxideHCID 16640769HCID 16640769, 화합물HCID 21226445Aluminium lithium hydride2회

생성물 1

HCID 21409913HCID 21409913, 화합물

시약·촉매·용매 2

HCID 962Water용매2회
HCID 3283
Diethyl Ether
용매
2회

실험 절차

2-Dimethylamino-2-methyl-propylamine dihydrochloride (2 g.) was dissolved in water (2 ml.) and the solution made alkaline with 5N sodium hydroxide. Chloroform (100 ml.) was added and the mixture was dried (anhyd. Na2SO4) and filtered. A solution of chloral (1.45 g.) in chloroform (50 ml.) was added to the stirred and cooled chloroform solution. The mixture was heated under reflux for 40 hrs., and the excess chloroform evaporated under reduced pressure to give an oily residue (0.9 g.). This was dissolved in ether (50ml.), the solution was added dropwise to a cooled and stirred suspension, of lithium aluminum hydride (0.43 g.) in ether (100 ml) and the mixture was heated under reflux for 16 hrs. On cooling, the excess lithium aluminum hydride was decomposed by the addition of water, and the mixture dried (anhydrous Na2SO4), and extracted with ether. The ether extracts were extracted with 2N HCl (2 × 20 ml. and 40 ml.), the excess water was evaporated under reduced pressure and the liquid residue dried by re-evaporation with ethanol/benzene mixture to give a solid residue. This was crystallised from ethanol to give N-methyl-2-dimethylamino-2-methyl propylamine dihydrochloride (0.9 g.)

후처리

  1. dry with materialthe mixture was dried (anhyd. Na2SO4)
  2. filtrationfiltered
  3. additionA solution of chloral (1.45 g.) in chloroform (50 ml.) was added to the
  4. temperaturecooled chloroform solution
  5. temperatureThe mixture was heated
  6. temperatureunder reflux for 40 hrs
  7. custom, and the excess chloroform evaporated under reduced pressure
  8. customto give an oily residue (0.9 g.)
  9. additionthe solution was added dropwise to
  10. temperaturea cooled
  11. stirringstirred suspension
  12. temperatureunder reflux for 16 hrs
  13. temperatureOn cooling
  14. dry with materialthe mixture dried (anhydrous Na2SO4)
  15. extractionextracted with ether
  16. extractionThe ether extracts were extracted with 2N HCl (2 × 20 ml. and 40 ml.)
  17. customthe excess water was evaporated under reduced pressure
  18. dry with materialthe liquid residue dried by re-evaporation with ethanol/benzene mixture
  19. customto give a solid residue
  20. customThis was crystallised from ethanol

출처 및 근거

ORD 기록
ord-1a50a14687bb4c8e8bed732aa98f48dd
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03975443

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