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求日本和俄羅斯關於如何制備1,3-二溴-5,5-二甲基海因的專利

日本和俄羅斯沒有它的制備專利,妳要求也不要太高。相關合成文獻基本都在下面了。

Process for producing N-halogenated hydantoins. Elnagar, Hassan Y.; Peters, Bruce C.; Spielman, Edgar E.; Thomas, Dustin H. (USA). 17 pp., US 2006036099

Preparation of dibromohydantoin bactericidal algaecides. Jiang, Yanyi. (Longkou Keda Chemical Co., Ltd., Peop. Rep. China). Faming Zhuanli Shenqing Gongkai Shuomingshu (2005), 6 pp. CN 1611493

Process for producing N-halogenated organic compounds. Elnagar, Hassan Y.; Peters, Bruce C.; Spielman, Edgar E.; Thomas, Dustin H. (USA). US 2005049420

Preparation of 2,4-dibromo-5,5-dimethylhydantoin aqueous solution disinfectant. Zhou, Li-xue; Zhu, Yun-qi. Xuzhou College of Industrial Technology, Xuzhou, Peop. Rep. China. Nanjing Gongye Daxue Xuebao, Ziran Kexueban (2004), 26(6), 36-40.

Method for preparing 1,3-dibromo-5,5-dimethylhydantoin granule for killing harmful bacteria in the cultivating water source. Huang, Zhongping. (Zhongshun Biotechnology Co., Ltd., Wuxi, Peop. Rep. China). Faming Zhuanli Shenqing Gongkai Shuomingshu (2003), 6 pp. CODEN: CNXXEV CN 1410363

Methods for microbiological control in aqueous systems. Howarth, Jonathan N.; Nalepa, Christopher J.; Sanders, Michael J. (Albemarle Corporation, USA). US 6641828

Study on synthesis and the antimicrobial activity of N,N-dihalo-5,5-dimethylhydantoin. Zhang, Shengli; Xu, Zuxun; Huang, Jingxia; Chen, Zuxing. Sch. Chem. Material Sci., Hubei Univ., Wuhan, Peop. Rep. China. Hubei Daxue Xuebao, Ziran Kexueban (2002), 24(1), 63-65.

Process for producing n-halogenated organic compounds. Elnagar, Hassan Y.; Peters, Bruce C.; Spielman, Edgar E., Jr.; Thomas, Dustin H. (Albemarle Corporation, USA). PCT Int. Appl. (2001), 55 pp. WO 2001053270

1,3-Dibromo-5,5-dimethylhydantoin of enhanced properties. Elnagar, Hassan Y.; Howarth, Jonathan N.; Peters, Bruce C.; Spielman, Edgar E., Jr.; Thomas, Dustin H. (Albemarle Corporation, USA). PCT Int. Appl. (2001), 31 pp. WO

Treatment of wastewater discharged from production of hydantoin's derivates. Huang, Jinxia; Yu, Guang'ao; Li, Rulan. Department of Chemistry, Hubei University, Wuhan, Peop. Rep. China. Jingxi Huagong (1998), 15(2), 55-58.

Compositions and methods utilizing 1,3-bromochloro-5-methyl-5-propylhydantoin. Bhattacharya, Bhabatosh. (Great Lakes Chemical Corporation, USA). PCT Int. Appl. (1997), 24 pp WO 9743264

New Aspects on the Preparation of 1,3-Dibromo-5,5-dimethylhydantoin. Markish, Itzhak; Arrad, Onn. CHEMADA, Doar Na Hanegev, Israel. Industrial & Engineering Chemistry Research (1995), 34(6), 2125-7. (這份應該是最接近工業生產,也應是最準確的)

Synthesis of 1,3-dibromo-5,5-dimethylhydantoin. Xu, Zhanghuang; Huang, Jinxia; Li, Yan; Fang, Guosu. Dep. Chem., Hubei Univ., Wuhan, Peop. Rep. China. Huaxue Shiji (1994), 16(5), 307-8, 311.

Organic synthesis using sodium bromate. II. A facile synthesis of N-bromo imides and amides using sodium bromate and hydrobromic acid (or sodium bromide) in the presence of sulfuric acid. Fujisaki, Shizuo; Hamura, Satoshi; Eguchi, Hisao; Nishida, Akiko. Fac. Eng., Yamaguchi Univ., Tokiwadai, Japan. Bulletin of the Chemical Society of Japan (1993), 66(8), 2426-8.

Densified halogenated dimethylhydantoins. Cole, Leon M. (Great Lakes Chemical Corp., USA). U.S. (1985), 5 pp. US 4532330

1,3-Dihalo-5,5-dialkylhydantoins. Bury, Zofia; Kwit, Daniela; Jaworska, Romana. (Instytut Farmaceutyczny). Pol. (1966), 2 pp. PL 51580

Abstract:

The title compds. prepd. by the known method are easily sepd. from reaction mixts. and in this way the yields of the compds. are much higher than those of the 5,5-dialkylhydantoins. The method described makes it possible to avoid acidification of the reaction mixt. and in this way to prevent HCN evolution. Thus, 120 g. NH4HCO3 is dissolved at 50? in 118 ml. 25% NH3, 50 ml. H2O, 35 g. KCN, and 37 ml. Me2CO are added, the mixt. is heated 2.5 hrs. under vigorous stirring at 55-60? and 3 hrs. at 90? and cooled to 15?. NaOH (42 g.) in 1000 ml. H2O is added, 57 ml. Br dropped in during 30 min., and the mixt. stirred at 10-15? 1.5 hrs. and kept overnight to crystallize at room temp. to give 100 g. yellow cryst. product m. 196-8?, contg. 99% 1,3-dibromo-5,5-dimethylhydantoin. 1,3-Dichloro-5,5-dimethylhydantoin, m. 130-2?, is obtained similarly.

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