반응 #803710

ord-d29ace45e3554fff8245c4da1b951547

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the volatile was concentrated in vacuo
  2. 2
    추출The aqueous layer was extracted with ethyl acetate
  3. 3
    건조the organic layer was dried over MgSO4
  4. 4
    여과filtered
  5. 5
    농축concentrated in vacuo

실험 절차

D-(−)-α-Phenylglycine (0.165 mmol) was dissolved in tetrahydrofuran (500 mL), followed by the addition of NaHCO3 (0.496 mmol) in water (500 mL), and then the addition of methylchloroformate (0.182 mmol) at room temperature. The reaction mixture was stirred at room temperature overnight. The mixture was acidified to pH=3 with HCl (1N) and the volatile was concentrated in vacuo. The aqueous layer was extracted with ethyl acetate and the organic layer was dried over MgSO4, filtered, and concentrated in vacuo to give compound 31 as a pale yellow solid in 80% yield. MS (ESI, EI+) m/z=209 (MH+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09187496B2uspto-grants-2015_11