تفاعل #7506

ord-ebdb6c09cb774332a0a1cecc00fe64cd

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىobtained
  2. 2
    درجة الحرارةcooled
  3. 3
    ترشيحfiltered over dicalite
  4. 4
    أخرىThe filtrate was separated into its layers
  5. 5
    غسيلThe organic layer was washed with H2O
  6. 6
    تجفيفdried (MgSO4)
  7. 7
    ترشيحfiltered
  8. 8
    أخرىthe solvent was evaporated
  9. 9
    أخرىThe residue was purified over silica gel on a glass
  10. 10
    ترشيحfilter (eluent: CH2Cl2/CH3OH 100/0 to 97/3)
  11. 11
    أخرىThe pure fractions were collected
  12. 12
    أخرىthe solvent was evaporated

الإجراء التجريبي

A mixture of 5,10-dihydro-imidazo[1,2-b]-isoquinoline-7,8-diol, obtained according to the procedure described in Ex.No. A8 c, (0.155 mol), phenyltrimethylammonium chloride (0.31 mol) and K2CO3 (0.68 mol) in DMF (400 ml) was stirred at 90° C. for 20 hours, cooled, poured out into H2O and filtered over dicalite. The filtrate was separated into its layers. The organic layer was washed with H2O, dried (MgSO4), filtered and the solvent was evaporated. The residue was purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 100/0 to 97/3). The pure fractions were collected and the solvent was evaporated, yielding 3 g of 5,10-dihydro-7,8-dimethoxyimidazo[1,2-b]isoquinoline (8.4%) (interm. 22).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07087595B2uspto-grants-2006_08