تفاعل #515330

ord-4e9b7e4c7d0c4359959afae045280f98

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAt the end of the reaction
  2. 2
    أخرىthe methanol is evaporated
  3. 3
    غسيلwashed with ethyl acetate
  4. 4
    استخلاصAfter extraction
  5. 5
    تجفيفdrying over MgSO4
  6. 6
    تركيزthe product is concentrated in vacuo
  7. 7
    أخرىPurification on a silica column
  8. 8
    أخرىto be obtained (eluant

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06313160B1uspto-grants-2001_11