Methanol → HCID 53798545, Verbindung

Temperatur

0 °C

A reactor was charged with 1 mole of 2-methyl-5-hydroxyimino-2-heptene, 8 moles of methanol containing 1.2 moles of sodium methylate, and 10 moles of tetrahydrofuran (THF). The mixture was cooled to 0° C., and with stirring, 1.3 moles of allyl bromide was added dropwise over 5 minutes. The mixture was stirred at room temperature for one day. The reaction mixture was concentrated, and 40 parts of methylene chloride was added. The mixture was washed with water, and the solvent was evaporated. The residue was purified by silica gel column chromatography to give 2-methyl-5-allyloxyimino-2-heptene in a yield of 80 mole %. Identification of this compound was performed by using IR, NMR and mass spectra (the same techniques were used to identify compounds appearing hereinafter).

1. stirringThe mixture was stirred at room temperature for one day
2. concentrationThe reaction mixture was concentrated
3. addition40 parts of methylene chloride was added
4. washThe mixture was washed with water
5. customthe solvent was evaporated
6. customThe residue was purified by silica gel column chromatography

ORD-Eintrag

ord-7475892712fd458aa88cf7d94d0c1dda

Quelldatensatz

uspto-grants-1990_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04906768