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
A mixture of 6.4 parts of 2,5-bis-trichloromethyl-1,3,4-thiadiazole and 30 parts by volume of 91% sulfuric acid is heated for 0.1 hour at from 175° to 185° C. The reaction mixture is then carefully poured on to ice and the precipitated solid is suction filtered. The product is washed with water and treated with 20 parts by volume of methanol, and small amounts of undissolved starting material are filtered off. After concentration of the methanolic solution there is obtained 3.4 parts (83% of theory) of 2-trichloromethyl-1,3,4-thiadiazole; m.p.: 58° C.
後処理
- temperatureis heated for 0.1 hour at from 175° to 185° C
- additionThe reaction mixture is then carefully poured on to ice
- filtrationfiltered
- washThe product is washed with water
- additiontreated with 20 parts by volume of methanol, and small amounts
- filtrationare filtered off
出典と根拠
- ORDレコード
- ord-d68bbce0e4fb402b87e7deda3a0cc99e
- 出典データセット
- uspto-grants-1978_04
- 特許番号
- US04083986
反応ノート
読み込み中…