Naphazoline hydrochloride synthesis
- Product Name:Naphazoline hydrochloride
- CAS Number:550-99-2
- Molecular formula:C14H14N2.ClH
- Molecular Weight:246.74
835-31-4
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Yield:550-99-2 92.33%
Reaction Conditions:
with hydrogenchloride in acetonitrile at 20;Large scale;Solvent;
Steps:
1.B-4.B; 1.C-4.C; 1.B-2.B; 1.C-2.C; 3-4
(B) naphazoline free base is dissolved in 8 L of acetonitrile,25% hydrochloric acid was added dropwise at room temperature, pH was adjusted to 2, and a solid was precipitated.The crude product of naphazoline hydrochloride was filtered, 1399.3 g.
(C) The crude product was added to the reaction vessel with 5 L of methanol and heated to 70 ° C.After the solution is dissolved, activated carbon is added, and the temperature is raised to 70 ° C to decolorize.After filtration, 1 L of acetone was added dropwise to the filtrate, the filtrate was cooled and cooled, and the crystal was incubated overnight at 25 ° C.Centrifugation, acetone rinsing, vacuum drying at 50 ° C for about 24 hours to obtain the finished naphazoline hydrochloride,White solid, 1366.6g,The yield was 92.33%, and the purity was 99.90% by HPLC.The bulk density is 0.49g/cm3,The angle of repose is 27°.The powder is loose and weak.
References:
Guangdong Xian Qiang Pharmaceutical Co., Ltd.;Guangdong Zhongsheng Pharmaceutical Co., Ltd.;Guangdong South China Pharmaceutical Group Co., Ltd.;Huang Caifeng;Li Wan;Xiong Weimei;Ye Qiongxian;Tan Zhenyou CN110041261, 2019, A Location in patent:Paragraph 0040; 0043-0044; 0045; 0048-0049; 0050; 0053-0054