HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyrazole → HCID 15672100, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyrazole | HCID 1048 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N-Methylsulfamoyl chloride | HCID 11789235 | — |
| Reactant | HCID 15672098 | HCID 15672098 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 15672100 | HCID 15672100 | 71.7% |
Reaction Steps
N-Methylaminosulfonyl chloride (0.22 g, 1.67 mmoles) was added dropwise to a solution of 3-(5-amino-2,4-dichlorophenyl)-4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazole (0.44 g, 1.28 mmoles) and triethylamine (0.17 g, 1.67 mmoles) in 20 ml anhydrous tetrahydrofuran under cooling with ice to react with the pyrazole derivative. After the addition was finished, the reaction was continued further for 2 hours. Then ethyl acetate was added to the reaction product solution, and the mixture was washed with water. The separated organic layer was dehydrated, concentrated, and purified by recrystallization from a n-hexane-ether mixture, giving the title compound (0.40 g), m.p. 133.0° C., yield 71.7%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05032165 |
| Source dataset | uspto-grants-1991_07 |
| ORD ID | ord-c75ac408c7fc43c19f1b995cea4d04df |
| Source note | uspto-grants-1991_07 |