Electric Literature of 4464-18-0 ,Some common heterocyclic compound, 4464-18-0, molecular formula is C9H12O3, its 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.
Preparation 2 1,3,5-Tris(bromomethyl)benzene A solution of thionyl bromide (3.1 mL, 8.3 g, 0.04 M) in chloroform (25 mL) is added dropwise over a period of 10 minutes to a stirred slurry of 1,3,5-tris(hydroxymethyl)-benzene (Preparation 1, 1.9 g, 0.012 M) in chloroform (100 mL). The mixture is stirred at room temperature for four hours during which the solids dissolve into solution. The solution is heated at reflux temperature for 45 minutes, cooled to room temperature, and examined by TLC which shows the reaction is complete. The chloroform and excess thionyl bromide are removed under reduced pressure, leaving a reddish-yellow solid residue. The crude product is chromatographed on a filtration column of gravity silica gel (63-200 mmu, 60 g) in methylene chloride. The column is eluted with methylene chloride and three fractions of 250 mL each are collected. The desired product is eluted in fraction 2 (4.13 g) and is recrystallized from hexane, giving the title compound (3.20 g) as colorless crystals, mp 95.5-97.5 C. W. Reppe and W. J. Schweckendiek, Justus Liebigs Ann. Chem., 560:1041 (1948) report amp of 94 C.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 4464-18-0, Benzene-1,3,5-triyltrimethanol, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; The Upjohn Company; US5500417; (1996); A;,
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