تفاعل #49039

ord-97c9716f95c14692a5ef32b3dbd750ba

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto warm gradually
  2. 2
    تركيزconcentrated under reduced pressure
  3. 3
    أخرىThe residue was roughly purified by silica gel column chromatography

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745663B2uspto-grants-2010_06