SU418038A1 - The method of obtaining-organosalicylthiophosphates - Google Patents

Description

the mixture is brought to room temperature, the solvent and volatiles are removed in vacuo and the product is isolated by distillation. Yield 90%; m.p. 167-169 ° C (1.5 mmHg); ng 1,5608; df 1.3761. MRn found 60.65; calculated 61.44. Found,%: P 12.36; S 12.20. CioHi, O4PS. Calculated,%: P 12,01; S 12.41. According to example 1, other salicylthiophosphates are obtained, the yield and some properties of which are listed in the table. Example 2. Getting 5-2,5-dichlorophenylsalicylate. A mixture of 0.05 g-mol salicylic acid and 0.055 g-mol phosphorus trichloride in 20 ml of dry chloroform was boiled for 3 hours. To the resulting solution of 20 ° C, 0.05 g-mol of glacial accelerated acid is added, and then at -20-10 ° C a solution of 0.05 g-mol 2.5 dichlorophenylsulfenyl chloride in 20 ml of chloroform. The mixture was brought to room temperature, the solvent and volatiles were removed in vacuo and the product was obtained as a residue. Yield 87%; m.p. -129 ° C (after washing with ether). Paydeno,%: C1 19.37; P 8.29; S 8.46. C, sN7C12O4P5. Calculated,%: C1 19.69; P 8.61; S 8.87. Example 3. Getting 5-phenylsalicylate. To 0.03 g-mol of thiophenol in 20 ml of chloroform at -20-10 ° C, 0.03 g-mol of sulfuryl chloride was added, the mixture was boiled for 30 minutes and solution A was prepared. To a mixture of 0.03 g-mol of salicylic chlorophosphite and 0.03 gmol of glacial acetic acid in 20 ml of chloroform at -40-30 ° C. solution A is added. The reaction mass is brought to room temperature, the solvent and volatiles are removed in vacuo, the residue is mixed with 5 ml of ether, the product is filtered and dried in vacuo. Yield 88%; m.p. 116-117 ° C. Found,%: P 10.36; S 10.64. Ci3H904PS. Calculated,%: P 10,61; S 10.95. In examples 1, 2 and 3, other salicylate thiophosphates are obtained, the yield and some properties of which are listed in the table.