تفاعل #356776

ord-7bcd6824560e4b9c9644522f7863956a

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwhile cooling (
  2. 2
    أخرىhighly exothermic reaction), and the reaction mixture
  3. 3
    workup.STIRRINGis stirred for a further 2 h
  4. 4
    أخرىAfter the separation of the phases
  5. 5
    غسيلthe organic phase is washed twice with water and once with a saturated aqueous sodium chloride solution
  6. 6
    تجفيفdried over sodium sulfate
  7. 7
    أخرىThe solvent is evaporated in vacuo
  8. 8
    أخرى31.8 g (93% of theory) of product are obtained

الإجراء التجريبي

100 ml of a 1M diisobutylaluminum hydride solution in dichloromethane are added to a solution, cooled to 0° C., of 33.98 g (100.5 mmol) of 2-benzyloxy-5-iodobenzaldehyde (Example 2A) in 200 ml of dichloromethane. After stirring at 0° C. for 2 h, a saturated potassium sodium tartrate solution is added while cooling (highly exothermic reaction), and the reaction mixture is stirred for a further 2 h. After the separation of the phases, the organic phase is washed twice with water and once with a saturated aqueous sodium chloride solution and dried over sodium sulfate. The solvent is evaporated in vacuo. 31.8 g (93% of theory) of product are obtained.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07446102B2uspto-grants-2008_11