Method for synthesizing 2-amido-6-chloropurine
A synthetic method, the technology of chloropurine, applied in the direction of organic chemistry, etc., can solve the problems of low product yield, difficulty in suction filtration, viscous material, etc., and achieve high yield and reasonable synthesis process
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Embodiment 1
[0045] Example 1 Synthesis of 2-amino-6-chloropurine (1)
[0046] The synthetic method of 2-amino-6-chloropurine (1) comprises the following steps successively:
[0047] a) Preparation of 2-dimethylaminomethenimino-6-chloropurine (3)
[0048] First add 40mL of N,N-dimethylformamide to the dry reaction bottle, and add 35mL of POCl dropwise at 0℃~10℃ 3 , formulated as POCl 3 N,N-dimethylformamide solution, set aside; then in another dry reaction bottle, add 200mL of 1,2-dichloroethane and 20g of guanine (2), at 20℃~30℃ , dropwise add the prepared N,N-dimethylformamide solution of phosphorus oxychloride. After dripping, keep stirring for 1 hour, then heat up and reflux for 5 to 8 hours to complete the reaction, and cool to obtain 2-dimethylaminomethenimino-6-chloropurine (3). The intermediate product (3) does not need to be obtained from the reaction solution Separated from, the reaction solution containing the intermediate product (3) is for subsequent use;
[0049] b) Prep...
Embodiment 2
[0056] The synthesis of embodiment two 2-amino-6-chloropurine (1)
[0057] The synthetic method of 2-amino-6-chloropurine (1) comprises the following steps:
[0058] a) Preparation of 2-dimethylaminomethenimino-6-chloropurine (3)
[0059] First add 40mL of N,N-dimethylformamide to the dry reaction bottle, and add 35mL of POCl dropwise at 0℃~10℃ 3 , formulated as POCl 3 N,N-dimethylformamide solution, set aside; then in another dry reaction bottle, add 200mL of 1,2-dichloroethane and 20g of guanine (2), at 20℃~30℃ , dropwise add the prepared N,N-dimethylformamide solution of phosphorus oxychloride. After dripping, keep stirring for 1 hour, then heat up and reflux for 5 to 8 hours to complete the reaction, and cool to obtain 2-dimethylaminomethenimino-6-chloropurine (3). The intermediate product (3) does not need to be prepared from the reaction solution Separated from, the reaction solution containing the intermediate product (3) is for subsequent use;
[0060] b) Preparat...
Embodiment 3
[0067] Example 3 Synthesis of 2-amino-6-chloropurine (1)
[0068] The synthetic method of 2-amino-6-chloropurine (1) comprises the following steps successively:
[0069] a) Preparation of 2-dimethylaminomethenimino-6-chloropurine (3)
[0070] First, add 40mL of N,N-dimethylformamide to the dry reaction bottle, and add 35mL of POCl dropwise at 0-10°C 3 , formulated as POCl 3 N,N-dimethylformamide solution, set aside; then in another dry reaction bottle, add 200mL of 1,2-dichloroethane and 20g of guanine (2), at 20℃~30℃ , dropwise add the prepared N,N-dimethylformamide solution of phosphorus oxychloride. After dripping, keep stirring for 1 hour, then heat up and reflux for 5 to 8 hours to complete the reaction, and cool to obtain 2-dimethylaminomethenimino-6-chloropurine (3). The intermediate product (3) does not need to be prepared from the reaction solution Separated from, the reaction solution containing the intermediate product (3) is for subsequent use;
[0071] b) Pre...
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