تفاعل #7506
ord-ebdb6c09cb774332a0a1cecc00fe64cd
معادلة التفاعل
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىobtained
- 2درجة الحرارةcooled
- 3ترشيحfiltered over dicalite
- 4أخرىThe filtrate was separated into its layers
- 5غسيلThe organic layer was washed with H2O
- 6تجفيفdried (MgSO4)
- 7ترشيحfiltered
- 8أخرىthe solvent was evaporated
- 9أخرىThe residue was purified over silica gel on a glass
- 10ترشيحfilter (eluent: CH2Cl2/CH3OH 100/0 to 97/3)
- 11أخرىThe pure fractions were collected
- 12أخرىthe 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).