반응 #58545

ord-7c7c8cff891047198df27509e2b94ac6

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with CH2Cl2 (300 ml)
  2. 2
    추출The organic extract
  3. 3
    건조was dried (MgSO4)
  4. 4
    기타purified by silica-gel chromatography

실험 절차

A solution of the product from step e) (4.38 g, 12.3 mmol) in CH2Cl2 (18.5 ml) was added dropwise to a slurry of AlCl3 (4.91 g, 36.9 mmol) in CH2Cl2 (42 ml) at 22° C. After 45 minutes, the reaction mixture was poured into ice cold 2 M NaOH (100 ml) and extracted with CH2Cl2 (300 ml). The organic extract was dried (MgSO4) and purified by silica-gel chromatography using a ethyl acetate/hexanes gradient (0% to 50% ethyl acetate) to give the subtitle product (434 mg, 12%). MS calculated for C17H17NOS+H 284, observed 284.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07423056B2uspto-grants-2008_09