تفاعل #72576

ord-09ecf914552d448a9062a9e77337ce31

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe catalyst is filtered off on a bed of Celite
  2. 2
    غسيلis then washed with acetic acid (20 ml)
  3. 3
    أخرىThe filtrate is evaporated to dryness
  4. 4
    أخرىthe residual acetic acid is removed by azeotropic distillation with toluene
  5. 5
    أخرىThe solid obtained
  6. 6
    أخرىis recrystallised from a mixture of EtOH/ethyl ether

الإجراء التجريبي

To a solution of the compound obtained in Step E (7.68 mmoles) in acetic acid (15 ml) there are added TFA (7 ml) and Pd/C 10% (400 mg). The reaction mixture is stirred at 50° C. under 4 bars of hydrogen overnight. The catalyst is filtered off on a bed of Celite and is then washed with acetic acid (20 ml). The filtrate is evaporated to dryness and the residual acetic acid is removed by azeotropic distillation with toluene. The solid obtained is recrystallised from a mixture of EtOH/ethyl ether to yield the title product after drying in vacuo.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541412B2uspto-grants-2013_09