تفاعل #219277

ord-daa05a7ddeb148df9d3a671b4d156bfb

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىby flushing with N2(g) for 30 min
  2. 2
    ترشيحfollowed by filtration
  3. 3
    غسيلan EtOAc rinse
  4. 4
    تجفيفThe organic layer was dried with MgSO4
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

An oven dried round-bottom flask was cooled to room temperature by flushing with N2(g) for 30 min. 1,4-Dioxa-spiro[4.5]decan-8-one (1.35 g, 8.66 mmol) (dissolved in 12 mL THF), 2-Methyl-propane-2-sulfinic acid amide (1.0 g, 8.25 mmol) (dissolved in THF), and titanium(IV) ethoxide (3.77 g, 16.50 mmol) were added. The reaction was stirred for 4 h at room temperature. To the mixture was added 15 mL saturated NaHCO3 followed by filtration and an EtOAc rinse. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure yielding 0.98 g of Compound 15.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07385085B2uspto-grants-2008_06