Reaktion #69264

ord-4d23c9e92ae44147a899cda23b71c32d

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    ExtraktionThe reaction was extracted with ethyl acetate
  2. 2
    Waschenthe organic extracts were washed with water, and saturated NaCl
  3. 3
    Trocknendried (MgSO4)
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigeThe crude product was used in the next reaction without further purification

Vorschrift

1,4-Dioxaspiro[4.5]decan-8-ol (0.40 g, 0.0025 mol) was dissolved in chloroform (10.0 mL) and the resulting mixture was cooled at 0° C. To the mixture was added TEA (0.49 mL, 0.0035 mol) and methanesulfonyl chloride (0.23 mL, 0.0030 mol) and this mixture was stirred at 0° C. for 2 hours. The reaction was extracted with ethyl acetate and the organic extracts were washed with water, and saturated NaCl, then dried (MgSO4) and concentrated in vacuo. The crude product was used in the next reaction without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08530485B2uspto-grants-2013_09