in neat (no solvent)
byproducts: H2, SMe2; to BH3*SMe2 at 0°C under Ar was added the amine, stirred until evolution of H2 had ceased, Me2S was removed at high vac., heated to 120°C over a period of 90 min, left for 1.5 h at this temp.; cooling, distn. under Ar;
The Board of Trustees of the University of Illinois; PsychoGenics, Inc.; Chandrasekhar, Jayaraman; Kozikowski, Alan P.; Liu, Jianhua; Tueckmantel, Werner; Walker, Joel R.; Yuen, Po-wai
Patent: US2013/184313 A1, 2013 ;
Location in patent: Paragraph 1179 ;
dihydrogen peroxide in tetrahydrofuran
under nitrogen, cooled at 0°C, after stirring for 45 min NaOH (3 M) and 30percent H2O2 added, stirred for 1 h, water added, saturated with K2CO3; aq. phase extn. (ether), combined org. phase dried, destn. under vacuum; NMR;
参考文献
Hill, E. Alexander; Park, Young-Whan
Journal of Organometallic Chemistry, 1988 , vol. 356, p. 1 - 16
