Formic Acid → N-[2-(7-methoxy-1,3-benzodioxol-5-yl)ethyl]formamide

HRID 1253109Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1253109
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:13][CH2:14][NH-:15])[CH:7]=[C:8]2[O:12][CH2:11][O:10][C:9]=12.[OH-].[Na+].[CH:18](O)=[O:19]>O>[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:13][CH2:14][NH:15][CH:18]=[O:19])[CH:7]=[C:8]2[O:12][CH2:11][O:10][C:9]=12

Komponenten

5

Edukt 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 867421922-(3-Methoxy-4,5-methylenedioxyphenyl)ethylamide hydrochloride

Produkt 1

HCID 10198394N-[2-(7-methoxy-1,3-benzodioxol-5-yl)ethyl]formamideAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

6.95 g (30 mmol) of 2-(3-methoxy-4,5-methylenedioxyphenyl)ethylamide hydrochloride was dissolved in 30 ml of water, and the mixture was made basic with 25% sodium hydroxide aqueous solution. The mixture was extracted with 30 ml of toluene. The toluene layer was washed with 10 ml of water, added with 2.73 g (59.3 mmol) of formic acid, refluxed under heating for 2 hours at normal pressure to distill off about 15 ml of the toluene while separating the produced water by an azeotropic distillation and then cooled. The deposited crystal was filtered out, washed with 3 ml of toluene and dried to obtain 5.48 g of N-[2-(3-methoxy-4,5-methylenedioxyphenyl)ethyl]formamide (C). Yield: 83%; melting point: 108°-110° C.

Aufarbeitung

  1. extractionThe mixture was extracted with 30 ml of toluene
  2. washThe toluene layer was washed with 10 ml of water
  3. temperaturerefluxed
  4. temperatureunder heating for 2 hours at normal pressure
  5. distillationto distill off about 15 ml of the toluene
  6. customwhile separating the produced water
  7. distillationby an azeotropic distillation
  8. temperaturecooled
  9. filtrationThe deposited crystal was filtered out
  10. washwashed with 3 ml of toluene
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0c793d2906a54f72b6fcb4757a104709
Quelldatensatz
uspto-grants-1988_05
Patentnummer
US04746747

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