Hydrochloric Acid → 3-Methoxyoct-1-yne

To an ice-cooled solution of 63 g. of 1-octyn-3-ol in 300 ml. of dimethoxyethane is added under an inert atmosphere 312 ml. of 1.6 M n-butyllithium in hexane dropwise over 1 hour. To the mixture is then added 145 g. of methyl iodide and the resulting mixture is stirred at ambient temperatures for 24 hours and then treated to 60° C. for 1 hour. The mixture is cooled and poured into cold dilute hydrochloric acid. The organic phase is separated, washed with water and saturated brine, dried (Na2SO4), and evaporated to an oil, dried (Na2SO4), and evaporated to an oil. Fractional distillation of the oil in vacuo yields the product as a colorless oil.

1. additionTo the mixture is then added 145 g
2. additiontreated to 60° C. for 1 hour
3. temperatureThe mixture is cooled
4. customThe organic phase is separated
5. washwashed with water and saturated brine
6. dry with materialdried (Na2SO4)
7. customevaporated to an oil
8. dry with materialdried (Na2SO4)
9. customevaporated to an oil
10. distillationFractional distillation of the oil in vacuo

ORDレコード

ord-a3cf842bc7dc4fcfa2b08270a2c3e423

出典データセット

uspto-grants-1978_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04123456