Hydrochloric Acid → HCID 20336130, Verbindung

HRID 1706503Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1706503
[H-].[Na+].[CH2:3]([O:5]C=O)[CH3:4].[CH3:8][C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:13])[C:10](=[O:12])C.Cl>CCOCC.C1C=CC=CC=1>[CH3:13][C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:8])[C:10](=[O:12])[CH2:4][CH:3]=[O:5]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 2854623-Methyl-3-phenylbutan-2-one

Produkt 1

HCID 20336130HCID 20336130, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittel3×HCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A mixture of 8.8 g. of 50% NaH oil dispersion in 150 ml. of dry benzene was treated at 25° C. with 13.6 g. of ethylformate in 20 ml. of dry benzene under N2. Over a period of a half hour, 14.9 g. of 3-methyl-3-phenyl-2-butanone in 80 ml. of dry benzene was added at 0° C. After stirring at 40° C. for 4 hours, the mixture was diluted with 250 ml. of ether, treated with ice and acidified with hydrochloric acid. The acidic solution ws extracted with ether and the ether extract was washed with brine, sodiuim bicarbonate solution, washed again with brine and dried. The solvent was evaporated and the residue was distilled under reduced pressure to afford 14.8 g. of the title product as an oil, B. P. 83°-84°/0.2 mm., λmaxfilm 3.5 (broad) 5.75, 5.90, 6.12, 6.30, 6.70, 6.80, 6.95, 7.31, 7.94, 8.18, 9,38, 12,60, 13.05 and 14.28 μ.

Aufarbeitung

  1. additionA mixture of 8.8 g
  2. waitOver a period of a half hour
  3. additionthe mixture was diluted with 250 ml
  4. extractionThe acidic solution ws extracted with ether
  5. extractionthe ether extract
  6. washwas washed with brine, sodiuim bicarbonate solution
  7. washwashed again with brine
  8. customdried
  9. customThe solvent was evaporated
  10. distillationthe residue was distilled under reduced pressure
  11. customto afford 14.8 g

Quellen und Nachweise

ORD-Eintrag
ord-75b86eea38344e03b53276e3cec65a0b
Quelldatensatz
uspto-grants-1980_06
Patentnummer
US04207419

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