Reference of 74137-36-3, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 74137-36-3 as follows.
[0353] A 1.6 M solution of n-butyllithium in hexane (5.65 niL, 9.04 mmol) was dissolved in dry toluene (50 mL) under dry argon and cooled to -5°C. Then a 2M solution of n-butylmagnesium chloride (2.26 mL , 4.52 mmol) was added slowly with the temperature held below 0°C over a period of 15 min. Stirring was continued for 45 min at -5°C, followed by drop wise addition of a solution of l,3-dibromo-5-methoxy-benzene (3.00 g, 11.3 mmol) in toluene (30 mL) with the temperature held below 00C. The mixture was stirred for 45 min at -5°C. A solution of iodine chloride (1.83 g, 11.3 mmol) in methylene chloride (20 mL) was added in the described manner and stirring continued for additional 20 min at -5°C. The mixture was warmed to room temperature. Water (50 mL) and toluene (50 mL) were added and the layers were separated. The organic layer was washed with a saturated aqueous solution OfNa2S2O3 (2 x 30 mL), water and brine (30 mL). The organic layer was dried (MgSO4) and concentrated to give the crude product which was purified by flash chromatography on silica gel (100 g, AcOEt/heptane 1:9). l-Bromo-3-iodo-5- methoxy-benzene (2.12 g, 60 percent) was obtained as a yellow oil, which crystallized quickly upon standing.
According to the analysis of related databases, 74137-36-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; LOCUS PHARMACEUTICALS, INC.; WO2008/8059; (2008); A1;,
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