تفاعل #54966

ord-e61af428fdb94cdeb327be221c10d5d9

الكواشف

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ظروف التفاعل

درجة الحرارة
171°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture is heated in the course of 45 minutes to 167° C
  2. 2
    workup.WAITstired for 1 hour
  3. 3
    ترشيحThe precipitated crystalline product is collected by filtration
  4. 4
    غسيلwashed with 350 ml of water
  5. 5
    أخرىThe 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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04151210uspto-grants-1979_04