تفاعل #54966
ord-e61af428fdb94cdeb327be221c10d5d9
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
171°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةthe mixture is heated in the course of 45 minutes to 167° C
- 2workup.WAITstired for 1 hour
- 3ترشيحThe precipitated crystalline product is collected by filtration
- 4غسيلwashed with 350 ml of water
- 5أخرىThe residue is dried at 25 torr and 50° C.
الإجراء التجريبي
A suspension of 22.7 g of sodium p-toluenesulphinate in 50 ml of dimethyl methanephosphonate is treated with 12.6 g of triethylamine and the mixture is heated in the course of 45 minutes to 167° C. The temperature is raised further to 171° C. and kept thereat for a further 30 minutes. The cooled solution is poured into 700 ml of water and stired for 1 hour. The precipitated crystalline product is collected by filtration and washed with 350 ml of water. The residue is dried at 25 torr and 50° C., affording 17.2 g (80.9% of theory) of p-tolylmethylsulphone of the formula ##STR14## with a melting point of 85°-96° C. and a purity of 95.8%.