* 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.
[00215] To a stirred solution of 1-bromo-2,4-dimethyl-3-nitro-benzene (2.66 g, 11. 6 mmol) in acetic acid (48 mL) was added iron (2.58 g, 46.3 mmol) and the mixture heated at 80°C for 18h, cooled and filtered. The filtrate was evaporated to dryness in vacuo and the residue basified with aqueous sodium hydroxide and then extracted with ethyl acetate 3x. The organicswere dried with magnesium sulfate and the solution evaporated to dryness in vacuo. The residue was purified by flash chromatography eluting with ethyl acetate 0-30percent in hexane to give3-bromo-2,6-dimethyl-aniline (1 .28 g, 6.40 mmol, 55.3percent)
42%
With hydrogenchloride; tin(ll) chloride In ethanol; water for 12 h; Reflux
[intermediate 11-a] (37.8g, 0.164mol), tin chloride (93.5g, 0.492mol), ethanol 500mL, hydrochloric acid 10mL, and water 10mL, was added and reflux. After 12 hours, the reaction mixture was then basified with aqueous solution of sodium hydroxide and the organic layer was separated by column chromatographyto give [Intermediate 11-b] 14 g (yield: 42percent).
Reference：
[1] Journal of Medicinal Chemistry, 2018, vol. 61, # 16, p. 7202 - 7217
[2] Patent: WO2015/79251, 2015, A1, . Location in patent: Paragraph 00215
[3] Patent: KR2015/124677, 2015, A, . Location in patent: Paragraph 0334; 0339-0342
[4] Patent: WO2009/44311, 2009, A1, . Location in patent: Page/Page column 39
2
[ 39053-43-5 ]
[ 7439-89-6 ]
[ 53874-26-3 ]
Reference：
[1] Patent: US2005/49286, 2005, A1,
3
[ 81-20-9 ]
[ 53874-26-3 ]
Reference：
[1] Patent: WO2015/79251, 2015, A1,
[2] Patent: KR2015/124677, 2015, A,
[3] Journal of Medicinal Chemistry, 2018, vol. 61, # 16, p. 7202 - 7217
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