2-CHLORO-4,5-DIAMINOPYRIMIDINE synthesis

Yield: 54.5%

Reaction Conditions:

with water;iron;ammonium chloride in ethanol at 100; for 4 h;

Steps:

21 Synthesis of Compound 21-3
To a solution of compound 21-2 (20 g, 114.6 mmol) in EtOH/H₂O (4/1, 400 mL) was added iron powder (64 g, 1146 mmol) and NH₄Cl (aq., 62 g, 1146 mmol), the reaction solution was stirred at 100° C. for 4 h, followed by filtration. The filter cake was washed with MeOH (10 mL×3) and the filtrate was concentrated to give compound 21-3 (9 g, Yield 54.5%) as yellow solid.

References:

Hubei Bio-Pharmaceutical Industrial Technological Institute Inc.;Humanwell Healthcare (Group) Co., Ltd.;Wang, Xuehai;Wu, Chengde;Xu, Yong;Shen, Chunli;Li, Li'e;Hu, Guoping;Yue, Yang;Li, Jian;Guo, Diliang;Shi, Nengyang;Huang, Lu;Chen, Shuhui;Tu, Ronghua;Yang, Zhongwen;Zhang, Xuwen;Xiao, Qiang;Tian, Hua;Yu, Yanping;Chen, Hailiang;Sun, Wenjie;He, Zhenyu;Shen, Jie;Yang, Jing;Tang, Jing;Zhou, Wen;Yu, Jing;Zhang, Yi;Liu, Quan US2017/313683, 2017, A1 Location in patent:Paragraph 0544