Trifluoroacetic acid → HCID 178513859, compound
Reaction equation
[C:1]([C:4]1[N:8](CC2C=CC(OC)=CC=2)[C:7]([SH:18])=[N:6][N:5]=1)(=[O:3])[NH2:2].FC(F)(F)C(O)=O.C1(OC)C=CC=CC=1>>[C:1]([C:4]1[N:8]=[C:7]([SH:18])[NH:6][N:5]=1)(=[O:3])[NH2:2]Participants
4
Procedure
3-Carbamoyl-4-(p-methoxybenzyl)-1,2,4-triazole-5-thiol (2.0 g., 0.007 mole), trifluoroacetic acid (8 ml.) and anisole (2 ml.) were heated at 70° C. for 3.5 hours. At this point, most of the trifluoroacetic acid present was removed by means of evaporation under reduced pressure and the residue was subsequently triturated with diethyl ether. The resulting solid was then filtered, washed with diethyl ether and subsequently dried in vacuo at 50° C. to give pure 3-carbamoyl-1,2,4-triazole-5-thiol (1.0 g., 91% yield), m.p. 276°-278° C. The infrared absorption spectrum was identical to that of a reference sample prepared as described in Example XVI, Part C.
Workup
- customAt this point, most of the trifluoroacetic acid present was removed by means of evaporation under reduced pressure
- customthe residue was subsequently triturated with diethyl ether
- filtrationThe resulting solid was then filtered
- washwashed with diethyl ether
- customsubsequently dried in vacuo at 50° C.
Sources & evidence
- ORD record
- ord-91b4a7fbe00f42d0807d9117388945a8
- Source dataset
- uspto-grants-1980_01
- Patent number
- US04183925
Reaction notes
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