반응 #795288

ord-93d8730cbb8345499cb59e46d93e85cd

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도under reflux for 3 hours
  3. 3
    농축The mixture was concentrated
  4. 4
    기타the residue purified on silica gel column
  5. 5
    세척eluting the product with 10% of methanol in dichloromethane

실험 절차

A mixture of 0.67 g (5.0 mmol) of 1-(1-hydroxy-2-methylpropan-2-yl)thiourea and 1.60 g (5.00 mmol) of 4,8-dibromo-3,4-dihydro-2Hbenzo[b]oxepin-5-one in 30 ml of ethanol was heated under reflux for 3 hours. The mixture was concentrated, the residue purified on silica gel column eluting the product with 10% of methanol in dichloromethane. Yield 1.38 g (75%). MS(ESI+): 369.3

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09175009B2uspto-grants-2015_11