Sulfuric Acid → 2-(Trichloromethyl)-1,3,4-thiadiazole
Reaction equation
[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]=1Participants
3
Procedure
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.
Workup
- 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
Sources & evidence
- ORD record
- ord-d68bbce0e4fb402b87e7deda3a0cc99e
- Source dataset
- uspto-grants-1978_04
- Patent number
- US04083986
Reaction notes
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