HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68535315, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | HCID 68540206 | HCID 68540206 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68535315 | HCID 68535315 | 96% |
Reaction Steps
Place 2-p-tolyl-5-trimethylsilanyl-2H-pyrazol-3-ylamine (170 mg, 0.693 mmol) in ethyl acetate (10 mL). Add potassium carbonate (191 mg, 1.38 mmol) and water (2 mL). Stir the reaction and add trichloroethyl chloroformate (0.114 mL, 0.831 mmol). Stir at room temperature for 18 hours. Add water and ethyl acetate. Separate organic layer and wash with saturated aq. sodium chloride. Collect organic layer, dry over Mg2SO4, filter, and concentrate under reduced pressure. Subject residue to silica gel chromatography eluting with 0-30% EtOAc:hexane to yield 280 mg (96%) of the title compound. MS(ES+): m/z=420.2 [M+H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652015B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-37e275c0e8a94250bb4b2f15aae55ccc |
| Source note | uspto-grants-2010_01 |