تفاعل #5995

ord-7bee3f2deba042d7930137633227fc6b

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISTILLATIONto distill off
  2. 2
    workup.ADDITIONAfter 1 hour (pot temperature =90° C.), 1N hydrochloric acid (35 mL) is added
  3. 3
    أخرىto precipitate a gum
  4. 4
    workup.ADDITIONOn addition of 10 mL of ether, crystals
  5. 5
    أخرىRecrystallization from ethyl acetate petroleum ether
  6. 6
    أخرىgives pure product

الإجراء التجريبي

A solution of 1.10 g (0.0019 mole) of the diester from Example 32 in 100 mL of methanol and 15 mL of 2N sodium hydroxide is heated to the boiling point, allowing the methanol to distill off. After 1 hour (pot temperature =90° C.), 1N hydrochloric acid (35 mL) is added to precipitate a gum. On addition of 10 mL of ether, crystals develop; wt. 0.84 g. Recrystallization from ethyl acetate petroleum ether gives pure product; mp 190°-192° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05246943uspto-grants-1993_09