HRID255539

反应详情

EQUATION

反应方程式

HRID 255539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. temperaturethe mixture was heated at its
  2. temperaturereflux temperature for two hours
  3. customEvaporation
  4. customprovided a residue which
  5. customseparated by filtration
  6. washwashed with water
  7. customRecrystallization from ethanol