반응 #494370

ord-e66369b1cc654ac4aa03ce335a60c17c

용매

반응 조건

온도
75°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was cooled to rt
  2. 2
    농축concentrated in vacuo to 50 mL
  3. 3
    추출extracted 3× with dichloromethane
  4. 4
    세척The combined organic fractions were washed 2× with water
  5. 5
    건조dried over sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated in vacuo

실험 절차

A solution of cyclohexene oxide (10.1 g, 103 mmol) and sodium azide (16.7 g, 257 mmol) in 100 mL of a 1:1 mixture of acetone:water was heated to reflux at 75° C. for 14 h. The mixture was cooled to rt, concentrated in vacuo to 50 mL, and extracted 3× with dichloromethane. The combined organic fractions were washed 2× with water, dried over sodium sulfate, filtered, and concentrated in vacuo to provide 2-azidocyclohexanol that gave a proton NMR spectra consistent with theory.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08754220B2uspto-grants-2014_06