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Trichloromethanesulfenyl chloride → 4-Phenyl-1,2-bis[(trichloromethyl)sulfanyl]-1,2,4-triazolidine-3,5-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trichloromethanesulfenyl chloride | HCID 11666 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Phenylurazole | HCID 85229 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Phenyl-1,2-bis[(trichloromethyl)sulfanyl]-1,2,4-triazolidine-3,5-dione | HCID 20356012 | — |
反応手順
To a solution of 35.4g (0.2 mole) 4-phenyl urazole in 200 ml water was added a solution of 16g (0.4 mole) sodium hydroxide in 20 ml water. A mixture of 74.4g (0.4 mole)trichloromethylsulfenyl chloride and 3g of an emulsifier solution (EXEM 25, consisting of a mixture of alkyl benzene sulfonate and ethoxylated vegetable oil) in 50 ml water was added dropwise to the above basic solution while keeping the reaction mixture at 0° C. The reactants were mixed so that the reaction mixture was kept at a pH greater than 7. The precipitate that formed was filtered and the filter cake was washed with water. After drying and recrystallizing from benzene there was obtained 4-phenyl-1,2-bis-(trichloromethylthio)urazole having a melting point of 175° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04087534 |
| 出典データセット | uspto-grants-1978_05 |
| ORD ID | ord-5e487487e6ed4ba898b9d3c8a62113dd |
| 出典メモ | uspto-grants-1978_05 |