Some common heterocyclic compound, 651734-54-2, name is 2,6-Difluoro-3,5-dimethoxyaniline, molecular formula is C8H9F2NO2, 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. HPLC of Formula: C8H9F2NO2
Example 1233-{ 13-(2,6-difluoro-3,5-dimethoxyphenyl)-2,8-dioxo-2,3,4,7,8,9-hexahydro-1H- pyrrolo j3?,2?:5,6j pyrido 14,3-d jpyrimidin-1-ylj methyl}benzonitrile Step 1: N-[(4-chloro-1-{[2-(trimethylsilyl)ethoxyJmethyl}-JH-pyrrolo[2, 3-bJpyridin-5- yl)methylJ-2, 6-dijluoro-3 , 5-dimethoxyaniline To a solution of sodium triacetoxyborohydride (6.2 g, 29 mmol) in trifluoroacetic acid (10.0 mL, 1.30E2 mmol) at 0 C was added a solution of 2,6-difluoro-3,5-dimethoxyaniline (1.52 g, 8.03 mmol) in methylene chloride (10 mL), followed by a solution of 4-chloro-1-{[2-(trimethylsilyl)ethoxy]methyl} -1 H-pyrrolo[2,3 -b]pyridine-5 -carbaldehyde (Example 106, Step 1: 2.27 g, 7.30 mmol) in methylene chloride (40 mL, 700 mmol). The reaction mixture was stirred at 0 C for 1 h then poured into a cold aqueous solution of NaHCO3 and then extracted with methylene chloride. The organic phase was washed with brine then dried over Na2SO4 and concentrated. The residue was purified by flash chromatography eluted with 0 to40 % EtOAc in DCM to give the desired product as a yellow oil which solidified on standing (3.32 g, 94 %). LC-MS calculated for C22H29C1F2N3O3Si (M+H) mlz: 484.2; found: 484.1.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 651734-54-2, its application will become more common.
Reference:
Patent; INCYTE CORPORATION; WU, Liangxing; ZHANG, Colin; HE, Chunhong; SUN, Yaping; LU, Liang; QIAN, Ding-Quan; XU, Meizhong; ZHUO, Jincong; YAO, Wenqing; WO2014/7951; (2014); A2;,
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