sodium hydrogen sulphate; 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 (10percent), NaHCO3 (10percent), H2O; mixt. warmed up to 200°C, then thermolysis at 800°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;