반응 #7506

반응 방정식

H2O

5,10-dihydro-imidazo[1,2-b]-isoquinoline-7,8-diol

K2CO3

DMF

→

5,10-dihydro-7,8-dimethoxyimidazo[1,2-b]isoquinoline

수율 8.4%

반응 조건

후처리

1. 1
   기타obtained
2. 2
   온도cooled
3. 3
   여과filtered over dicalite
4. 4
   기타The filtrate was separated into its layers
5. 5
   세척The organic layer was washed with H2O
6. 6
   건조dried (MgSO4)
7. 7
   여과filtered
8. 8
   기타the solvent was evaporated
9. 9
   기타The residue was purified over silica gel on a glass
10. 10
    여과filter (eluent: CH2Cl2/CH3OH 100/0 to 97/3)
11. 11
    기타The pure fractions were collected
12. 12
    기타the solvent was evaporated

실험 절차

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).

출처