Реакция #69343

ord-5d6e3ec387d34890bc6beb155f34c05e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe solvent is removed at reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
  3. 3
    Промывкаwashed with water
  4. 4
    ДругоеThe organic layer is dried
  5. 5
    Другоеthe solvent is removed

Методика

To an ice cooled solution of 5.31 g sodium nitrite and 8 g dried phloroglucinol in 70 ml dimethyl formamide is added a solution of 11.3 g 2-iodo-3-methyl-butyric acid ethyl ester in 30 ml dimethyl formamide. The solution is allowed to warm up to room temperature and is stirred over night. The solvent is removed at reduced pressure. The residue is dissolved in ethyl acetate and washed with water. The organic layer is dried and the solvent is removed. The title compound is obtained as an oil. MS: m/z (M+)=176.1

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08530493B2uspto-grants-2013_09