In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 39989-43-0, name is 3,5-Dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C7H7Cl2N
Dichlorobenzylamine (117 mg) was added to a solution of intermediate 36 (180 mg) in drydichloroethane (5 mL) under a Nitrogen atmosphere. After stirring for 1 h at r. t. NaBH (OAc) 3 (169 mg) was added and the resulting mixture was stirred at r. t. overnight. Then it was diluted with DCM, washed with an aqueous saturated sodium hydrogen carbonate solution, dried and concentrated in vacuo to give a crude oil, which was purified by flash chromatography (Biotage Flash 25M, CH/AcOEt 4: 1). The two fractions corresponding to products with Rf=0.36 and Rf=0.50 (CH/AcOEt 1: 1, detection with ninhydrine) were collected to give, after evaporation, an oil (40 mg) which was then dissolved, under a Nitrogen atmosphere, in dry MeOH (5 mL) and to which sodium methoxide (4.5 mg) was added. The mixture was refluxed for 5 h, then it was allowed to cool to r. t. and solvent was removed in vacuo. The residue was dissolved in AcOEt, washed with an aqueous saturated sodium hydrogen carbonate solution, dried and concentrated in vacuo. The crude product thus obtained was purified by flash chromatography (CH/AcOEt 9: 1) to give the title compound (35 mg) as a colourless oil. T. I. c.: CH/AcOEt 1: 1, Rf=0.5 (detection with ninhydrine). NMR(CDCI3) :6 (ppm) 7.31 (dd, 2H); 7.2 (t,1H) ; 6.98 (t, 2H); 6.83 (d, 2H); 4.25 (d,1H) ; 4.04 (d, 1H) ; 3.76 (b, 2H); 3.01 (td, 1H) ; 2.88 (m, 1H) ; 2.82 (bm, 1H) ; 2.63 (dd, 1H) ; 2.41 (b, 1H) ; 2.18 (bd, 1H) ; 2.05-2. 15 (m, 2H); 1.94 (b, 1H) ; 1.81 (b, 1H) ; 1.69 (m, 1H) ; 1.4 (s, 9H). MS (ES/+): m/z=543 [M+Na] +.
The synthetic route of 39989-43-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXO GROUP LIMITED; WO2005/49600; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics