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Sodium Carbonate → 5-Amino-5-methylheptan-3-one

HRID 839995
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 839995
C(C1(C)N=[C:7]([CH2:9][CH3:10])[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4]1)C.C(=O)([O-])[O-:16].[Na+].[Na+]>Cl>[NH2:4][C:5]([CH3:11])([CH2:12][CH3:13])[CH2:6][C:7](=[O:16])[CH2:9][CH3:10]
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Komponenten

4

Edukt 2

HCID 10340Sodium CarbonateHCID 205278902,4,6-Triethyl-2,6-dimethyl-1,2,5,6-tetrahydropyrimidine

Produkt 1

HCID 213304575-Amino-5-methylheptan-3-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

196.3 g of 2,4,6-triethyl-2,6-dimethyl-1,2,5,6-tetrahydropyrimidine were added dropwise to 300 ml of concentrated hydrochloric acid at 30° - 40° C, with stirring. When the addition was complete, the mixture was stirred for a further 4 - 5 hours and then neutralized with sodium carbonate and extracted with benzene. The resulting benzene solution was washed with, in turn, a 5% aqueous solution of sodium carbonate and water, and was then dried over potassium carbonate. After removal of benzene, the residue was distilled under reduced pressure, giving 72.4 g of 5-amino-5-methyl-3-heptanone (bp 46° - 48° C/2.5 mmHg).

Aufarbeitung

  1. additionWhen the addition
  2. stirringthe mixture was stirred for a further 4 - 5 hours
  3. extractionextracted with benzene
  4. washThe resulting benzene solution was washed with, in turn
  5. dry with materiala 5% aqueous solution of sodium carbonate and water, and was then dried over potassium carbonate
  6. customAfter removal of benzene
  7. distillationthe residue was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-26d4840fd9a34dd684296857809976ea
Quelldatensatz
uspto-grants-1978_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04097587

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