Formaldehyde → isopropyl N-(methylaminomethyl)carbamate hydrochloride

HRID 2049494

Reaktionsgleichung

Reaktionsgleichung von HRID 2049494
[ClH:1].[CH3:2][NH2:3].[CH2:4]=O.[C:6](=[O:12])([O:8][CH:9]([CH3:11])[CH3:10])[NH2:7]>C(O)C>[ClH:1].[CH3:2][NH:3][CH2:4][NH:7][C:6](=[O:12])[O:8][CH:9]([CH3:11])[CH3:10]

Komponenten

5

Edukt 3

HCID 712FormaldehydeHCID 15628Isopropyl carbamateHCID 6364545Methylamine hydrochloride

Produkt 1

HCID 12511010isopropyl N-(methylaminomethyl)carbamate hydrochlorideAusbeute 77,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

To 50 ml of ethanol, 20.3 g (0.3 mole) of methylamine hydrochloride and 30.9 g (0.36 mole) of 37% formaldehyde aqueous solution were added and the mixture was warmed to 35°-40° C. Then, a solution prepared by dissolving 30.9 g (0.3 mole) of isopropyl carbamate in 150 ml of ethanol was added dropwise to the mixture with stirring maintaining the said temperature. After the dropwise addition of the solution, stirring was continued for 1 hour with heating and then the solvent was removed by distillation under reduced pressure. The residue was recrystallized from ethanol to give 42.7 g of isopropyl N-(methylaminomethyl)carbamate hydrochloride having a melting point of 163°-164° C. in yield of 77.8%. ##STR5##

Aufarbeitung

  1. temperaturethe mixture was warmed to 35°-40° C
  2. customThen, a solution prepared
  3. additionwas added dropwise to the mixture
  4. temperaturemaintaining the said temperature
  5. additionAfter the dropwise addition of the solution
  6. stirringstirring
  7. temperaturewith heating
  8. customthe solvent was removed by distillation under reduced pressure
  9. customThe residue was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-280fc069745e431a8d0dd3daa014f1cd
Quelldatensatz
uspto-grants-1980_04
Patentnummer
US04197410

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