반응 #691095

ord-00a960acb4124e9db5ade53abf3de7aa

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for seven hours
  2. 2
    온도cooled at an icebath
  3. 3
    기타the phases were separated
  4. 4
    추출The aqueous layer was extracted with diethyl ether (200 mL)
  5. 5
    세척the combined organic layers were washed with brine (200 mL)
  6. 6
    건조dried (MgSO4)
  7. 7
    농축concentrated

실험 절차

Ethyl 2-mercaptoacetate (9.68 mL, 88.3 mmol) was added dropwise to a suspension of K2CO3 (12.2 g, 88.3 mmol) and 1-(1,3-benzodioxol-5-yl)-2-bromoethanone (21.4 g, 88.3 mmol) in dry acetone (100 mL). The mixture was stirred at reflux for seven hours, cooled at an icebath and added 200 mL water. Diethyl ether (400 mL) was added and the phases were separated. The aqueous layer was extracted with diethyl ether (200 mL) and the combined organic layers were washed with brine (200 mL), dried (MgSO4) and concentrated. This afforded the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07906502B2uspto-grants-2011_03