반응 #1100574

ord-68142354ff474a6ebd4b19f8023b011b

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), solvent
  4. 4
    기타evaporated in vacuo and residue
  5. 5
    기타purified by silica-gel chromatography

실험 절차

A solution of the product from step e) (4.9 g, 13.8 mmol) in CH2Cl2 (21 ml) was added dropwise to a slurry of AlCl3 (5.51 g, 41.4 mmol) in CH2Cl2 (47 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), solvent evaporated in vacuo and residue purified by silica-gel chromatography using a ethyl acetate/hexanes gradient (0% to 50% ethyl acetate) to give the subtitle compound (1.8 g, 46%). MS calculated for C17H17NOS+H 284, observed 284.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07981919B2uspto-grants-2011_07