反応 #49039

ord-97c9716f95c14692a5ef32b3dbd750ba

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to warm gradually
  2. 2
    濃縮concentrated under reduced pressure
  3. 3
    その他The residue was roughly purified by silica gel column chromatography

実験手順

To methyl hydroxypivalate (1.31 g, 9.89 mmol) were added tetrahydrofuran (40 ml), hydroxyphthalimide (3.23 g, 19.78 mmol) and triphenylphosphine (6.48 g, 24.73 mmol). After this solution was cooled to 0° C., diisopropyl azodicarboxylate (4.87 ml, 24.73 mmol) was added dropwise to the solution. While being allowed to warm gradually, the reaction mixture was stirred for 12 hours, and concentrated under reduced pressure. The residue was roughly purified by silica gel column chromatography to give the title compound (922 mg).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745663B2uspto-grants-2010_06