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Chloroform → HCID 21409913、化合物

HRID 2072003
ノート
印刷プレビュー

反応式

HRID 2072003 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6212ChloroformHCID 14798Sodium HydroxideHCID 16640769HCID 16640769、化合物HCID 21226445Aluminium lithium hydride2 回

生成物 1

HCID 21409913HCID 21409913、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回
HCID 3283
Diethyl Ether
溶媒
2 回

実験手順

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 aluminium hydride (0.43 g.) in ether (100 ml) and the mixture was heated under reflux for 16 hrs. On cooling, the excess lithium aluminium 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 NCl (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.)

後処理

  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 NCl (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

出典と根拠

ORDレコード
ord-4a86759b906349a4af3cb35f2325b526
出典データセット
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04049663

反応ノート

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