Sodium methanol solutions, physical

This would not be necessary nowadays as the preparation and resolution of 8 is an undergraduate experiment.5 A more normal reductive amination gives racemic 8 and crystallisation of the tartrate salt 12 from methanol gives enantiomerically pure (+)-(R)-S after neutralisation. In fact this nearly perfect resolution gives both enantiomers of 8. One tartrate salt crystallises out from MeOH and the other remains in solution. The salts are diastereoisomers and have different physical properties. Since no covalent bond is formed in making the salt 12, simple neutralisation with NaOH gives pure amine 8 and the tartaric acid remains in solution as its sodium salt. 

Cu-Zn-Cr oxides were prepared as follows. CuO was added to an aqueous solution of CrOj, and ZnO was added after 1 h aging. The obtained paste was dried without heating. Fe-based catalysts were prepared by the coprecipitation of the corresponding nitrates using sodium hydroxide. The precipitate was washed five times, dried at 120 C for 6 h and calcined at SSO C for 3 h. The composite catalysts were obtained by the physical mixing of the equal amounts of a methanol synthesis catalyst and a zeolite. HY [JRC-Z-HY4.8(2)] and NaY(JRC-Z-Y4.8) were provided from the Catalysis Society of Japan as the Reference Catalyst. 

Open-tubular column Soda-lime glass capillaries were treated with a sodium hydroxide aqueous solution at 45-50 "C for 2 days and washed with methanol until the effluent became neutral. The capillaries were then dried under helium at 120 "C for a few hours and washed with methanollc 0.01 H hydrochloric acid, water and methanol. Finally, the capillaries were dried mder helium at 120 °C for a few hours. Chemically and physically stable silica gel layer was formed on the glass surface with above pretreatments. An orgwic solution of octadecyltriethoxysilane was filled into the pretreated capillaries and the reaction weis carried out at elevated temperature. After the reaction, columns were washed with orgcuiic solvents and the mobile phase. Both ends of columns were inserted into narrow-bore(ca. 0.2 mm i.d.) PTFE tubing for small dead-volume connection. 

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