HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Bis{5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)pyrazol-4-yl}disulfide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)-4-thiocyanato pyrazole | HCID 15540354 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Bis{5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)pyrazol-4-yl}disulfide | HCID 18354787 | 55% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)-4-thiocyanatopyrazole 1.00 g (2.37 mmol) was dissolved in 20 ml of dry methanol, and then 210 mg (5.00 mmol) of 90% sodium borohydride was added at 0° C. After the mixture was was stirred at 0° C. for 3.5 hrs, the reaction mixture was poured into 80 ml iced water, and then the precipitate was collected by filtration. After drying in vacuo, the resulting yellow crystal was recrystalized from ethyl acetate-n-hexane mixed solvent to obtain 512 mg (0.65 mmol) of the title compound as a yellow crystal. Yield 55%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06316477B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-2d6dc178cc0749db85c97e55976d0047 |
| Source note | uspto-grants-2001_11 |