تفاعل #69961

ord-0037591a615e4fe095b275a6c05ed8ab

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto cool down to room temperature
  2. 2
    workup.WAITleft
  3. 3
    تركيزThe reaction mixture is concentrated under reduced pressure
  4. 4
    workup.DISSOLUTIONdissolved in ethyl acetate (200 ml)
  5. 5
    غسيلwashed with aqueous 2N sodium carbonate (100 ml)
  6. 6
    تجفيفThe organic layer is then dried over magnesium sulphate
  7. 7
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

To a suspension of 10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (9.97 g, 60 mmol) in methanol (200 ml) is added sodium tetrachloroaurate (597 mg, 1.5 mmol) and the reaction mixture is heated to 60° C. for 7 hours. The reaction mixture is allowed to cool down to room temperature and left to stand overnight. The reaction mixture is concentrated under reduced pressure, dissolved in ethyl acetate (200 ml) and washed with aqueous 2N sodium carbonate (100 ml), followed by saturated brine (100 ml). The organic layer is then dried over magnesium sulphate and concentrated under reduced pressure to give 5-methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (8.62 g)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530667B2uspto-grants-2013_09