Preparation of m-trifluoromethylaniline from benzotrifluoride by nitration and normal pressure catalytic hydrogenation. Wang,
Yanyong; Yang, Dongpeng; Zhang, Hongpeng; Zhou, Liming; Guong, Xiaoping. The Chemical Research Institute, Institute of Chemical Defence of CPLA,
Beijing, Peop. Rep. China. Jingxi Shiyou Huagong (2003), (1), 40-43. Publisher: Jingxi Shiyou Huagong Bianjibu, CODEN: JSHIBF ISSN:
1003-9384. Journal written in Chinese. CAN 141:227195 AN 2004:31056 CAPLUS
Abstract: m-Trifluoromethylaniline was prepd. from benzotrifluoride (phCF3) by nitration and normal pressure catalytic hydrogenation. The purity was
above 99% and the total yield reached to 89%. The optimum ratio of nitrating agent is PhCF3:HNO3:H2SO4 = 1:1.05:1.3(mol), the purity and yield of
m-trifluoromethyl nitrobenzene were 98.0% and 90.7% resp. The optimum conditions of catalytic hydrogenation are as follows: wt. of 5% Pd/C catalyst
used in the substrate = 2%, trifluoromethylnitrobenzene:abs. ethanol = 0.10 mol:100 mL, reaction temp. 45°, stirring speed 240 r/min, the purity and
the yield of m-trifluoromethylaniline were 99.3% and 98.5% resp.
Process for the mononitration of benzotrifluorides. Lobo, Marcos Souza; Scholze, Jakson Goi; Araujo, Marcelo Aguiar; Alvares, Paulo
Sergio Martins; Rahmeier, Luis Henrique Sanfelice. (Milenia Agro Ciencias S.A., Brazil). Braz. Pedido PI (2002), 8 pp. CODEN: BPXXDX BR
2000002090 A 20020102 Patent written in Portuguese. Application: BR 2000-2090 20000510. Priority: . CAN 137:169311 AN 2002:669748
CAPLUS
Abstract: Benzotrifluorides 4-XC6H4CF3 (X = H, Cl, F, Br, iodo) underwent mononitration to give 4,3-X(O2N)C6H3CF3 by treatment with 65-98% HNO3 in
excess (1.1:1 to 4:1 molar ratio) in the absence of a solvent at 0-150 for 1-18 h. Thus, nitration of p-chlorobenzotrifluoride using 3-fold
moles 98% HNO3 for 3 h at 90 afforded 95% 3-nitro-4-chlorobenzotrifluoride (purity 98%). |