Technology Process of Stannane, tributyl(6-methyl-1-cyclohexen-1-yl)-
There total 5 articles about Stannane, tributyl(6-methyl-1-cyclohexen-1-yl)- which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
gas;
byproducts: hexabutylditin; placing starting material in a porcelain cup in the sublimation chamber of a flash vac. thermolysis apparatus, react. at 800-850°C in the main oven and 250-300°C in the sublimation oven (10E-2 mm), oven packed with broken porcelain; vapors quenched on a dewar cold finger, pyrolysis tube cooled to room temp., product washed with ether from the dewar surface, ether evapd., chromy. (florisil);
- Guidance literature:
-
In
gas;
byproducts: hexabutylditin; placing starting material in a porcelain cup in the sublimation chamber of a flash vac. thermolysis apparatus, react. at 800-850°C in the main oven and 250-300°C in the sublimation oven (10E-2 mm), oven packed with broken porcelain; vapors quenched on a dewar cold finger, pyrolysis tube cooled to room temp., product washed with ether from the dewar surface, ether evapd., chromy. (florisil);
- Guidance literature:
-
With
sodium hydrogen sulfate; sulfuric acid; water;
In
pyridine; dichloromethane;
byproducts: p-H3CC6H4OH; slow addn. of soln. of CH3PhOC(S)Cl in CH2Cl2 to cold (-20°C) soln. of alcohol in pyridine, 3h. 0°C, ice, extd. with CH2Cl2, treatment with H2SO4 (10%), NaHCO3 (10%), H2O; mixt. warmed up to 200°C, then thermolysis at 750°C; in N2, condensation of products in a dewar vessel (liquid N2), warmed up to ambient temp.; first reaction detected by HPLC and IR, purifn. of educt by chromy. (Florisil, pentane), purifn. checked by HPLC or GC;
DOI:10.1016/0022-328X(87)80020-7
