Preparation method of 4-chloropyrrolo[2,3-d]pyrimidine
A technology of chloropyrrolopyrimidine and hydroxypyrrolopyrimidine, which is applied in the field of chemical synthesis, can solve the problems of 4-chloropyrrolopyrimidine, such as unsafe hazards, and achieve the effects of reduced synthesis cost, safe and reliable synthesis process, and short production cycle
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Embodiment 1
[0040] (1) Synthesis of 2-mercapto, 4-amino, 6-hydroxypyrimidine
[0041] Dissolve ethyl cyanoacetate and thiourea in ethanol at a molar ratio of 1:1, slowly add sodium ethoxide that is 1.5 times the molar weight of ethyl cyanoacetate at 0°C, stir at room temperature for 2 hours, then raise the temperature to 85°C, and reflux the reaction After 8 hours, cool to room temperature, filter, wash the solid with ethanol, and dry to obtain 2-mercapto, 4-amino, 6-hydroxypyrimidine in a yield of 85%.
[0042] (2) Synthesis of 4-amino, 6-hydroxypyrimidine
[0043] Add 2-mercapto, 4-amino, and 6-hydroxypyrimidine to ammonia water with a mass concentration of 25%, and the amount of ammonia is 10 times the mass of 2-mercapto, 4-amino, and 6-hydroxypyrimidine; then add 2-mercapto , 4-amino, active nickel with 3 times the molar weight of 6-hydroxypyrimidine, heated to 80 ° C, refluxed for 6 hours, then filtered while hot to remove active nickel, cooled to room temperature, precipitated soli...
Embodiment 2
[0050] (1) Synthesis of 2-mercapto, 4-amino, 6-hydroxypyrimidine
[0051] Dissolve ethyl cyanoacetate and thiourea in ethanol at a molar ratio of 1:3, slowly add sodium ethoxide that is twice the molar amount of ethyl cyanoacetate at 5°C, stir at room temperature for 3 hours, then raise the temperature to 90°C, and reflux the reaction After 9 hours, cool to room temperature, filter, wash the solid with ethanol, and dry to obtain 2-mercapto, 4-amino, 6-hydroxypyrimidine in a yield of 80%.
[0052] (2) Synthesis of 4-amino, 6-hydroxypyrimidine
[0053] Add 2-mercapto, 4-amino, and 6-hydroxypyrimidine to ammonia water with a mass concentration of 20%, and the amount of ammonia is 15 times the mass of 2-mercapto, 4-amino, and 6-hydroxypyrimidine; then add 2-mercapto , 4-amino, 6-hydroxypyrimidine mole to that 4 times the active nickel, heated to 80 ° C, refluxed for 6 hours, then filtered to remove the active nickel while hot, cooled to room temperature, precipitated solid, filte...
Embodiment 3
[0060] (1) Synthesis of 2-mercapto, 4-amino, 6-hydroxypyrimidine
[0061] Dissolve ethyl cyanoacetate and thiourea in ethanol at a molar ratio of 1:2, slowly add sodium ethoxide that is 2.5 times the molar weight of ethyl cyanoacetate at 0°C, stir at room temperature for 1.5 hours, then raise the temperature to 90°C, and reflux the reaction After 10 hours, cool to room temperature, filter, wash the solid with ethanol, and dry to obtain 2-mercapto, 4-amino, 6-hydroxypyrimidine in a yield of 82%.
[0062] (2) Synthesis of 4-amino, 6-hydroxypyrimidine
[0063] 2-mercapto, 4-amino, and 6-hydroxypyrimidine are added to ammonia water with a mass concentration of 25%, and the amount of ammonia is 20 times the mass of 2-mercapto, 4-amino, and 6-hydroxypyrimidine; then add 2-mercapto , 4-amino, 6-hydroxypyrimidine mole to that 6 times the active nickel, heated to 80 ° C, refluxed for 6 hours, then filtered while hot to remove active nickel, cooled to room temperature, precipitated sol...
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