반응 #548428

ord-d16a47a2217547bbbe3ccf38e98a7f6f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 18 hours
  2. 2
    온도The reaction mixture is cooled
  3. 3
    여과filtered
  4. 4
    농축concentrated
  5. 5
    기타The residue is partitioned between ether and water
  6. 6
    추출The aqueous phase is extracted several times with ether
  7. 7
    세척The extract is washed with sodium bisulfite solution, water and saline
  8. 8
    건조The organic solution is dried over magnesium sulfate
  9. 9
    농축concentrated
  10. 10
    기타to give 4.182 g
  11. 11
    workup.DISTILLATIONThe material is purified by distillation, b.p. 86°-87° C. (0.18 Torr)

실험 절차

To a solution of 3.57 g. (0.0162 mole) of ethyl 3,3-dimethyl-7-chloroheptanoate in 100 ml. of methyl ethyl ketone is added 4 g. of sodium iodide and the mixture heated at reflux for 18 hours. The reaction mixture is cooled, filtered and concentrated. The residue is partitioned between ether and water. The aqueous phase is extracted several times with ether. The extract is washed with sodium bisulfite solution, water and saline. The organic solution is dried over magnesium sulfate and concentrated to give 4.182 g. of a yellow oil. The material is purified by distillation, b.p. 86°-87° C. (0.18 Torr).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04061672uspto-grants-1977_12