반응 #93445

ord-d4de8aeca9ca45eda5bfc5d0c2ea9d50

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture is heated at 50°-55° C. for six hours
  2. 2
    기타retained at 60°-65° C.
  3. 3
    기타purified by flash chromatography
  4. 4
    기타The product is isolated from solution
  5. 5
    workup.DISTILLATIONby distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours

실험 절차

8.48 Grams of mesityl oxide (0.084 moles) is added dropwise to a solution of 21.0 grams of 2,6 di-tert-butyl-4-mercaptophenol (0.088 moles) and one gram of triethylamine in 30 ml of toluene. The mixture is heated at 50°-55° C. for six hours. The solvent is then stripped off under vacuum and the residue retained at 60°-65° C. and 0.20 mm. Hg. for two hours. The residue is dissolved in toluene and purified by flash chromatography using silica gel. The product is isolated from solution by distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04612341uspto-grants-1986_09