반응 #2191495

ord-e9bb8667c9064dc48adc204629e5d661

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe mixture was stirred for 16 h
  2. 2
    기타The organic layer was isolated
  3. 3
    추출The aqueous phase was extracted with diethyl ether (200 ml)
  4. 4
    기타The formed precipitation
  5. 5
    여과was filtered off
  6. 6
    세척washed with water
  7. 7
    기타dried in vacuo

실험 절차

An 1 N aqueous solution of lithium hydroxide (227 ml, 227 mmol) was added to a solution of 2-oxo-1-azaspiro[3.3]heptane-1-carboxylic acid tert-butylester (48 g, 0.227 mmol) in tetrahydrofuran (200 ml). The reaction mixture was stirred for 2 h. Diethyl ether (200 ml) and water (200 ml) were added. The mixture was stirred for 16 h. The organic layer was isolated. The aqueous phase was extracted with diethyl ether (200 ml). The aqueous phase was acidified with a 10% aqueous solution of sodium hydrogen sulfate until pH 3. The formed precipitation was filtered off, washed with water, and dried in vacuo, to give 38.84 g of (1-(tert-butoxycarbonylamino)cyclobutyl)acetic acid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07576062B2uspto-grants-2009_08