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Trichloromethanesulfenyl chloride → 4-(3-Chlorophenyl)-1,2-bis-(trichloromethylthio) urazole
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-(3-Chlorophenyl)-1,2,4-triazolidine-3,5-dione | HCID 1285521 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(3-Chlorophenyl)-1,2-bis-(trichloromethylthio) urazole | HCID 20356007 | — |
反応手順
To a solution of 42.2g (0.2 mole) 4-(3-chlorophenyl) 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 (as in example 1) 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 cyclohexane there was obtained 70g (69%) 4-(3-chlorophenyl)-1,2-bis-(trichloromethylthio) urazole having a melting point of 153° 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-8e2eb88ab11d40b1a7e10e885feceab1 |
| 出典メモ | uspto-grants-1978_05 |