تفاعل #44992

ord-ab216d039f774c28b387c1ba8123978c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe reaction solution is concentrated under reduced pressure
  2. 2
    workup.ADDITIONThe residue is diluted with ice-water
  3. 3
    غسيلwashed with diethyl ether
  4. 4
    استخلاصextracted twice chloroform
  5. 5
    غسيلThe organic layer is washed with saturated brine
  6. 6
    تجفيفdried over sodium sulfate
  7. 7
    تركيزThe solvent is concentrated under reduced pressure
  8. 8
    ترشيحcollected by filtration

الإجراء التجريبي

Methyl trans-4-(pyrrolidin-1-ylcarbonyl)cyclohexanecarboxylate (11.7 g) obtained in Reference Example 81(1) is dissolved in methanol (50 ml), and thereto is added a solution of sodium hydroxide (3.95 g) in water (20 ml). The mixture is then stirred at room temperature for 18 hours. The reaction solution is concentrated under reduced pressure. The residue is diluted with ice-water and washed with diethyl ether. The resulting aqueous layer is acidified with 10% hydrochloric acid and extracted twice chloroform. The organic layer is washed with saturated brine and dried over sodium sulfate. The solvent is concentrated under reduced pressure. The resulting residue is suspended in n-hexane and collected by filtration to give the title compound (10.1 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737161B2uspto-grants-2010_06