반응 #342721

반응 방정식

3,4-diaminoquinoline

acetic acid

water

N-carbomethoxy-S-methylisothiourea

→

methyl 1H-imidazo[4,5-c]quinolin-2-carbamate hydrate

용매

ethanol

ethanol

반응 조건

후처리

1. 1
   온도the mixture was heated at its
2. 2
   온도reflux temperature for two hours
3. 3
   기타Evaporation
4. 4
   기타provided a residue which
5. 5
   기타separated by filtration
6. 6
   세척washed with water
7. 7
   기타Recrystallization from ethanol

실험 절차

To a solution of 6.6 g (0.041 mole) of 3,4-diaminoquinoline (from Example 39), 2.0 ml of glacial acetic acid, 35 cc of ethanol and 35 ml of water was added 9.3 g (0.045 mole) of N-carbomethoxy-S-methylisothiourea, and the mixture was heated at its reflux temperature for two hours. Evaporation provided a residue which was suspended in ethanol, separated by filtration and washed with water. Recrystallization from ethanol provided methyl 1H-imidazo[4,5-c]quinolin-2-carbamate hydrate, m.p. >250° C. Analysis: Calculated for C12H10N4O2. 0.75H2O: %C, 56.4; %H, 4.5; %N, 21.9; Found: %C, 56.1; %H, 4.4; %N, 22.4.

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