反応 #69343

ord-5d6e3ec387d34890bc6beb155f34c05e

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent is removed at reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
  3. 3
    洗浄washed with water
  4. 4
    その他The organic layer is dried
  5. 5
    その他the solvent is removed

実験手順

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

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530493B2uspto-grants-2013_09