تفاعل #93028

ord-1c0bf66e0455439ea5f32903983ce016

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirred for two-hours
  2. 2
    workup.STIRRINGthe resulting solution was stirred for an hour
  3. 3
    غسيلthe separated organic layer was washed in turn with a saturated aqueous solution of sodium bicarbonate and brine
  4. 4
    أخرىdried
  5. 5
    أخرىThe solvent was evaporated

الإجراء التجريبي

Pyridine (0.39 ml) was added to a suspension of phosphorus pentachloride (1.01 ml) in dry methylene chloride (25 ml) at 5° C., and the mixture was stirred at ambient temperature for 30 minutes. Benzhydryl 7-phenylacetamido-3-(2,2-dibromovinyl)-3-cephem-4-carboxylate (2.5 g) was added to the above mixture at -10° C. and stirred for two-hours. Then, methylcellosolve (2.3 ml) was added to the reaction mixture at -30° C. and the resulting solution was stirred for an hour. To the above solution was added 5 ml of water and the separated organic layer was washed in turn with a saturated aqueous solution of sodium bicarbonate and brine, dried. The solvent was evaporated to give benzhydryl 7-amino-3-(2,2-dibromovinyl)-3-cephem-4-carboxylate (1.7 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04609730uspto-grants-1986_09