Реакция #668891

ord-9112fb2b129e47a0bf6980c11e82861e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONare added slowly dropwise
  2. 2
    workup.STIRRINGafter which the mixture is stirred for a further 60 minutes
  3. 3
    Температураwithout cooling
  4. 4
    Экстракцияis subjected to extraction with diethyl ether
  5. 5
    Сушкаthe organic phase is dried over sodium sulfate
  6. 6
    Фильтрацияthe drying agent is filtered off
  7. 7
    Другоеevaporation of the solvent

Методика

9.3 g (0.11 mol) of cyclopentanone and 13.5 g (0.11 mol) of methyl 2-chloropropionate are cooled to 0 to 2° C.; at this temperature, 13.6 g (0.12 mol) of potassium tert-butylate suspended in 200 ml of tetrahydrofuran are added slowly dropwise with stirring over a period of about 90 minutes, after which the mixture is stirred for a further 60 minutes without cooling. A little water is added to the reaction mixture, which is subjected to extraction with diethyl ether; the organic phase is dried over sodium sulfate, the drying agent is filtered off, and evaporation of the solvent gives 10.6 g of methyl 2-methyl-1-oxaspiro[2.4]heptane-2-carboxylate, which can be employed without further purification in the subsequent stage (see b).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05922648uspto-grants-1999_07