반응 #515330

ord-4e9b7e4c7d0c4359959afae045280f98

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타At the end of the reaction
  2. 2
    기타the methanol is evaporated
  3. 3
    세척washed with ethyl acetate
  4. 4
    추출After extraction
  5. 5
    건조drying over MgSO4
  6. 6
    농축the product is concentrated in vacuo
  7. 7
    기타Purification on a silica column
  8. 8
    기타to be obtained (eluant

실험 절차

1 g of 2,3-dihydro-1,4-benzodioxin-6-yl acetate (5.149 mmol) is dissolved in a solution of methanol (7.5 ml) and, under an argon atmosphere, the mixture is made basic, dropwise, with a 10% sodium hydroxide solution. The mixture is stirred at ambient temperature for 4 hours. At the end of the reaction, the methanol is evaporated and the reaction medium is acidified (to pH=1) with a 2N HCl solution and then washed with ethyl acetate. After extraction, drying over MgSO4 is carried out and the product is concentrated in vacuo. Purification on a silica column allows an oil to be obtained (eluant:PE/AcOEt 8/2 then 7/3).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06313160B1uspto-grants-2001_11