| 摘要 |
O,O-Dialkylthionophosphoric acid chlorides of the formula (RO)2P(S)Cl in which R represents a C1 to C6 alkyl radical, are obtained by reacting a suspension of P2S5 in an inert solvent at a temperature of from about 0 to 150 DEG C. with Cl2 and a C1 to C6 alkanol by introducing into the said suspension a stream of chlorine and adding dropwise concurrently the said alcohol, allowing the chlorination reaction to proceed to completion, expelling the solvent from the reaction mixture and isolating the O,O-dialkylthionophosphoric acid chloride by distillation. The preferred mole ratio of P2S5 to alcohol to chlorine is 1:4.0 to 4.4:2.2 to 3.2. It is also preferred that the chlorine and alcohol are introduced to the P2S5 suspension at a feed rate of approximately 1:2 (molar). The balance of chlorine is then introduced at a constant feed rate. Specified inert solvents are toluene, xylene, carbon tetrachloride, petroleum ether (boiling point 65-95 DEG C.) and the O,O-dialkylthionophosphoric acid chloride obtained as the reaction product. Specified alcohols are methanol, ethanol, n-propanol, iso-propanol, n-butanol, iso-butanol, amyl alcohol, hexyl alcohol and the isomers thereof. The chlorine used in the reaction may be diluted with inert gas such as CO2, A and N2 in a ratio by volume of about 1:0.5 to 1:3. The product may be purified by steam distillation. |
