تفاعل #939033

ord-7a309612a73f478487bc80aaed6533eb

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto obtain a solution
  2. 2
    workup.ADDITIONwas added
  3. 3
    أخرىreacted at 40° C. for 3 hours under nitrogen current
  4. 4
    استخلاصThe solution was extracted by ethyl acetate
  5. 5
    غسيلthe extracted liquid was washed with saturated salt water three times
  6. 6
    أخرىThe washed product was dried
  7. 7
    تركيزconcentrated by anhydrous magnesium sulfate
  8. 8
    أخرىrecrystallized by diethyl ether

الإجراء التجريبي

Potassium hydroxide 0.4 g was dissolved in ethanol 5 mL and dimethyl sulfoxide 200 mL was further added to obtain a solution. Benzoin methyl ether 30 g (0.13 mol) was dissolved in the solution and paraformaldehyde 5 g (0.16 mol) was added and reacted at 40° C. for 3 hours under nitrogen current. After that, the reaction product was cooled to a room temperature and neutralized with a dilute hydrochloric acid and then saturated salt water 120 mL was added. The solution was extracted by ethyl acetate and the extracted liquid was washed with saturated salt water three times. The washed product was dried and concentrated by anhydrous magnesium sulfate and recrystallized by diethyl ether. α-methylol benzoin methyl ether (MBME) was obtained in such a manner.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07253131B2uspto-grants-2007_08