반응 #734223

ord-4b6d210cd53b40b5b38d329f7bc3495c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONThe methanol was distilled off under reduced pressure
  2. 2
    기타the residue was recrystallized from hexane-diethyl ether

실험 절차

9-(2'-Hydroxy-3',4'-dimethoxy-6'-methylbenzoyl)nonanoic acid (formula II-1 wherein R=H3CO, X=H, Y=OH, n=8, in the free form) (0.197 part) was dissolved in methanol saturated with hydrogen chloride gas (7 volume parts) and the solution was stirred at room temperature for 20 minutes. The methanol was distilled off under reduced pressure and the residue was recrystallized from hexane-diethyl ether. The procedure provided methyl 9-(2'-hydroxy-3',4'-dimethoxy-6'-methylbenzoyl)nonanoate (formula II-1 wherein R=H3CO, X=H, Y=OH, n=8, in the form of methyl ester) (0.195 part) as colorless needles melting at 49°-53° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04407757uspto-grants-1983_10