Hydrochloric Acid → 1-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-1-methylhydrazine

HRID 335410Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 335410
[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:21])[C:13]([N:15]([CH3:20])[N:16]=C(C)C)=[O:14])[CH3:2].Cl>O1CCCC1>[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:21])[C:13]([N:15]([CH3:20])[NH2:16])=[O:14])[CH3:2]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 866893431-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(1-methylethylidene)hydrazine

Produkt 1

HCID 569428781-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-1-methylhydrazineAusbeute 68,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a 500 ml volume four-necked flask, 1-[(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(1-methylethylidene)hydrazine (18-a) (21.41 g) and tetrahydrofuran (150 ml) were added under a nitrogen atmosphere at room temperature. To the mixture, 10% by weight of hydrochloric acid (29.23 g) was added dropwise over 5 minutes, and stirred at room temperature for 1 hour. Then, the reaction mixture was concentrated under reduced pressure. To the residue was added water (80 ml), and extracted with tert-butyl methyl ether. The organic layer was concentrated under reduced pressure, and added hexane (50 ml). The precipitated crystal was collected by filtration and dried to give 12.70 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methylhydrazine ((12-2)-(11)-39).

Aufarbeitung

  1. concentrationThen, the reaction mixture was concentrated under reduced pressure
  2. additionTo the residue was added water (80 ml)
  3. extractionextracted with tert-butyl methyl ether
  4. concentrationThe organic layer was concentrated under reduced pressure
  5. additionadded hexane (50 ml)
  6. filtrationThe precipitated crystal was collected by filtration
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-be6c972810a748b695a1b0dc878b9912
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08884010B2

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