반응 #355783

ord-037be1b1b0ef41ba93b21ed6ef1338dd

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the reaction was concentrated in vacuo
  2. 2
    기타the residue partitioned between ethyl acetate (100 mL) and 2M hydrochloric acid (150 mL)
  3. 3
    기타The organic phase was separated
  4. 4
    세척washed with 1M aqueous sodium carbonate solution
  5. 5
    건조dried over sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated in vacuo

실험 절차

To a stirred solution of 4-(methylthio)benzoic acid (6.76 g, 40.2 mmol) and N-[2-(dimethylamino)ethyl]-N′-ethylcarbodiimide hydrochloride (9.24 g, 48.2 mmol) in THF (100 mL) was added morpholine (4.2 mL, 48.2 mmol). After stirring for 2 hours, the reaction was concentrated in vacuo and the residue partitioned between ethyl acetate (100 mL) and 2M hydrochloric acid (150 mL). The organic phase was separated, washed with 1M aqueous sodium carbonate solution, dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound LC retention time 3.52 mins MS m/z 238 (MH+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07446117B2uspto-grants-2008_11