* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With ammonium carbonate In N,N-dimethyl-formamide at 90℃;
Synthesis of 153-1. A solution of 153-0 (2.00 g, 8.4 mmol) and (NH4) 2CO3 (4.00 g, 42 mmol) in DMF (20 mL) was heated to 90 °C overnight. The mixture was cooled to room temperature and poured into water (100 mL). The precipitate was filtered off and washed with the mixture of diethyl ether (Et2O) and petroleum ether (PE; Et2O : PE = 1:1) to give 153-1 (1.50 g, 76 percent) as a yellow solid.
73%
With ammonia In methanol at 60℃; for 18 h; Sealed tube
A solution of 1-bromo-2,5-difluoro-4-nitrobenzene (2 g, 8.43 mmol) inmethanolic ammonia (25 mL) was heated at 60°C in a sealed tube, for 18h. The reactionwas concentrated in vacuo, and the residue purified by column chromatography (Si02, 0-30 percent EtOAc/hexanes), yielding the title compound as a yellow solid (1.4 g, 73percent). 1HNMR (400 MHz, CDC13) 7.90 (d, 1H), 7.10 (d, 1H), 5.98 (bs, 2H).
Reference：
[1] Patent: WO2017/7756, 2017, A1, . Location in patent: Paragraph 199
[2] Patent: WO2015/86525, 2015, A1, . Location in patent: Page/Page column 124
[3] Journal of Medicinal Chemistry, 2008, vol. 51, # 17, p. 5243 - 5263
[4] Patent: WO2009/134750, 2009, A1, . Location in patent: Page/Page column 131
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