Water → p-Tolyl methyl sulfone

HRID 26688

反応式

HRID 26688 の反応式
[C:1]1([CH3:10])[CH:6]=[CH:5][C:4]([S:7]([O-:9])=[O:8])=[CH:3][CH:2]=1.[Na+].[CH2:12](N(CC)CC)C.O>CP(OC)(=O)OC>[C:1]1([CH3:10])[CH:6]=[CH:5][C:4]([S:7]([CH3:12])(=[O:9])=[O:8])=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 962WaterHCID 8471TriethylamineHCID 2723791Sodium p-toluenesulfinate

生成物 1

HCID 18521p-Tolyl methyl sulfone収率 81.1%

試薬・触媒・溶媒 1

HCID 12958Dimethyl methylphosphonate溶媒

反応条件

温度
171 °C

実験手順

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%.

後処理

  1. temperaturethe mixture is heated in the course of 45 minutes to 167° C
  2. waitstired for 1 hour
  3. filtrationThe precipitated crystalline product is collected by filtration
  4. washwashed with 350 ml of water
  5. customThe residue is dried at 25 torr and 50° C.

出典と根拠

ORDレコード
ord-e61af428fdb94cdeb327be221c10d5d9
出典データセット
uspto-grants-1979_04
特許番号
US04151210

関連ノート

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