Allison, Brett D.; Hack, Michael D.; Phuong, Victor K.; Rabinowitz, Michael H.; Rosen, Mark D.
Patent: US2005/38032 A1, 2005 ;
Location in patent: Page/Page column 29 ;
US 20050038032 A1
1: anhydrous 1-octyne With n-butyllithium in tetrahydrofuran; hexane T=0°C; 2: With zinc dibromide in tetrahydrofuran; hexane T=0°C; 3: 4-cyanotoluene With n-tridecane; [NiCl2(PMe3)2] in tetrahydrofuran T=65°C; 46 h; Further stages.;
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sodium amide T=150°C; anschliessend Behandeln mit Wasser; Isolierung als Carbonat;
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1.1: copper(I) bromide / tetrahydrofuran; 2-methyl tetrahydrofuran / 4 h / 0 - 60 °C / Inert atmosphere 1.2: 0 °C / Inert atmosphere 1.3: 1 h / Inert atmosphere; Reflux 2.1: n-butyllithium / tetrahydrofuran; hexane / 0 °C / Inert atmosphere 2.2: 3.83 h / -78 - 20 °C / Inert atmosphere 3.1: 5 Pd(II)/C(eggshell); hydrogen / ethanol / 18 h / 45 °C / 3040.2 Torr View Scheme
参考文献
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