반응 #410058

ord-3ba37cce7b7d4a3497a10cae57bd6450

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도is heated
  2. 2
    온도at reflux for 40 hours
  3. 3
    기타The mixture is evaporated to dryness
  4. 4
    기타the residue is partitioned between ethyl acetate (200 mL) and water (200 mL)
  5. 5
    건조The organic layer is dried over magnesium sulphate
  6. 6
    여과filtered
  7. 7
    농축concentrated in vacuo
  8. 8
    세척Flash chromatography of the resulting oil, eluting with a mixture of ethyl acetate and cyclohexane (1:19 v/v)

실험 절차

A mixture of 3-benzyloxyphenol (3 g), ethyl (RS)-4-chloro-4-phenylbutanoate (4.53 g), potassium carbonate (4.14 g), potassium iodide (100 mg) and methyl ethyl ketone (100 mL) is heated at reflux for 40 hours. The mixture is evaporated to dryness and the residue is partitioned between ethyl acetate (200 mL) and water (200 mL). The organic layer is dried over magnesium sulphate, filtered, and concentrated in vacuo. Flash chromatography of the resulting oil, eluting with a mixture of ethyl acetate and cyclohexane (1:19 v/v), gives ethyl (RS)-4-(3-benzyloxyphenoxy)-4-phenylbutanoate (1 g), in the form of a yellow oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06211234B1uspto-grants-2001_04