Synthetic Route of 29671-92-9,Some common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, molecular formula is CH4Cl2N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Method A: 2,4-diamino-6-chloropyrido[3,2-c/]pyrimidine (7.5 g, 38 mmole), e.g. prepared according to Colbry et a/. J. Heterocycl, Chem. (1984) 21 :1521 , was suspended in 6 N HCI (300 ml) and the mixture was refluxed for 5 hours. After cooling, the pH was made alkaline (pH about 9 – 10) by means of 10 N NaOH. The precipitate obtained was filtered, washed with H2O and dried at 100 0C, resulting in the pure title compound (7.0 g, yield 95 %) which was characterized by its mass spectrum as follows: MS (m/z): 197 ([M+H]+, 100).Method B: A mixture of 3-amino-6-chloro-pyridine-2-carboxamide (5.1 g, 30 mmol), chloroform-amidine hydrochloride (6.99 g, 60 mmol), dimethylsulfone (24 g) and sulfolane (2.4 ml) was heated at 165 0C for 30 min. To the hot mixture was added water (50 ml). After cooling to room temperature, a diluted ammonium hydroxide solution was slowly added drop wise till pH 7. The resulting precipitate was filtered off, washed with water and dried overnight at 100 0C to give the pure title compound (5.8 g, 98 %). The obtained compound was used as such for further reactions without additional purification. M. p. >330C; elemental analysis calc. for C7H5CIN4O (196.6): C 42.77 H 2.56 N 28.50. Found: C 41.61 H 2.74 N 28.76.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Carbamimidic chloride hydrochloride, its application will become more common.
Reference:
Patent; 4 AZA Bioscience nv; WO2006/135993; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics