تفاعل #213925

ord-0e1524980eb44ce4880e7ae85a87aa21

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةfinally is heated
  2. 2
    درجة الحرارةat reflux for 60 min
  3. 3
    تركيزconcentrated
  4. 4
    أخرىThe residue is partitioned between ether and water
  5. 5
    غسيلThe ether layer is washed with water and brine
  6. 6
    تجفيفdried over MgSO4
  7. 7
    تركيزconcentrated
  8. 8
    workup.DISTILLATIONThe residue is subjected to fractional distillation
  9. 9
    أخرىto provide a light amber liquid, bp. 165°-180° (0.15 mm)

الإجراء التجريبي

To a stirred, ice-cold solution of sodium ethoxide in ethanol (prepared from 5.98 g of sodium spheres and 175 ml of ethanol) is added a solution of 29.8 g of thiophenol in 30 ml of ethanol during 15 min. After 10 min. this solution is treated at 0°-15° with a solution of 79.5 g of diethyl α-bromosuberate in 70 ml of ethanol during 15 min. The stirred mixture is warmed to room temperature during 60 min. and finally is heated at reflux for 60 min. The cooled solution is treated with 3 ml of gl acetic acid and concentrated. The residue is partitioned between ether and water. The ether layer is washed with water and brine, dried over MgSO4, and concentrated. The residue is subjected to fractional distillation to provide a light amber liquid, bp. 165°-180° (0.15 mm).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04254036uspto-grants-1981_03