Sulfuric Acid → 2-(Trichloromethyl)-1,3,4-thiadiazole
反応式
[Cl:1][C:2]([Cl:13])([Cl:12])[C:3]1[S:4][C:5](C(Cl)(Cl)Cl)=[N:6][N:7]=1.S(=O)(=O)(O)O>>[Cl:1][C:2]([Cl:13])([Cl:12])[C:3]1[S:4][CH:5]=[N:6][N:7]=1参加物
3
実験手順
6.4 parts by weight of 2,5-bis-trichloromethyl-1,3,4-thiadiazole is heated in 30 parts by volume of 91% sulfuric acid for 6 minutes at 175° to 185° C. The reaction mixture is subsequently poured carefully on to ice and the precipitated solid is filtered off. The reaction product is washed with water and treated with 20 parts by volume of methanol, and the minor amounts of undissolved starting material are filtered off. Concentration of the methanolic solution gives 3.4 parts (83% of theory) of 2-trichloromethyl-1,3,4-thiadiazole having a melting point of 58° C.
後処理
- additionThe reaction mixture is subsequently poured carefully on to ice
- filtrationthe precipitated solid is filtered off
- washThe reaction product is washed with water
- additiontreated with 20 parts by volume of methanol
- filtrationare filtered off
出典と根拠
- ORDレコード
- ord-797aee6e2b724ad3b0b420e404547833
- 出典データセット
- uspto-grants-1978_01
- 特許番号
- US04066775
反応ノート
読み込み中…