تفاعل #62236

ord-bdb5c2efb4434099bfacdae154ddb13a

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
45°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONThe reaction mixture was then poured into a 1000 mL beaker
  2. 2
    workup.STIRRINGstirred well until all the product
  3. 3
    أخرىwas precipitated out
  4. 4
    ترشيحThe tan colored product was then filtered
  5. 5
    غسيلwashed with water
  6. 6
    أخرىdried under vacuum

الإجراء التجريبي

A mixture of 75 g of polyphosphoric acid (Acros), 1,2,3-trimethoxybenzene (5.0 g, 29.73 mmol), and mono-methyl succinate (5.9 g, 44.59 mmol) were mechanically stirred at 45° C. for 2.5 h. The reaction mixture was then poured into a 1000 mL beaker containing round 250 mL of ice, and stirred well until all the product was precipitated out. The tan colored product was then filtered and washed with water and dried under vacuum. 6.1 g (72%) of 55 was obtained, which was pure by NMR.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07429681B2uspto-grants-2008_09