تفاعل #40528

ord-56dffb8badf046c4b6812a170c7583af

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe reaction stirred at room temperature 3 days
  2. 2
    تركيزThe pale yellow solution was concentrated
  3. 3
    أخرىto afford an oily residue, which
  4. 4
    أخرىwas triturated with ether
  5. 5
    ترشيحThe solids were collected by suction filtration
  6. 6
    أخرىdried in vacuo

الإجراء التجريبي

The 3,3-dimethyl-4-oxo-piperidine-1-carboxylic acid tert-butyl ester thus prepared (450 mg, 1.97 mmol) was dissolved in methylene chloride (10 mL). Trifluoroacetic acid was added (305 uL) and the resulting solution stirred at room temperature 2 h. Additional trifluoroacetic acid was added (300 uL) and the reaction stirred at room temperature 3 days. The pale yellow solution was concentrated to afford an oily residue, which was triturated with ether. The solids were collected by suction filtration and dried in vacuo. 3,3-Dimethyl-piperidin-4-one was isolated and used as its trifluoroacetic acid salt (381 mg, 80%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07727985B2uspto-grants-2010_06