HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 53850736, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyrazole | HCID 1048 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 22981229 | HCID 22981229 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 53850736 | HCID 53850736 | 73% |
Reaction Steps
Sodium hydride (0.54 g) was added to a mixture of pyrazole (1.0 g) and dimethyl sulfoxide (50 ml) under cooling with ice. The reaction mixture was stirred for 1 hour under cooling with ice and then a solution of N-(2-fluoro-5-nitrophenylmethyl)iminodicarboxylic acid di-tert-butyl ester (5.0 g) in dimethyl sulfoxide (50 ml) was added. The reaction mixture was stirred at room temperature for 15 hours and then water was added and extraction with ethyl acetate was conducted. The organic layer was washed with brine, dried with anhydrous sodium sulfate and then concentrated at reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:4) to give the titled compound (yield, 73%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06414005B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-cae7be939ce8448aafed9f036e4611cb |
| Source note | uspto-grants-2002_07 |