HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloride methanol → HCID 178508049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloride methanol | HCID 21893726 | — |
| Reactant | tert-butyl 5-(5-chloro-2-cyclopropoxyphenyl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-4-ylcarbamate | HCID 66852002 | — |
| Reactant | Tert-butyl 3-(5-chloro-2-cyclopropoxyphenyl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-4-ylcarbamate | HCID 70496613 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178508049 | HCID 178508049 | — |
Reaction Steps
Tert-butyl 3-(5-chloro-2-cyclopropoxyphenyl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-4-ylcarbamate and tert-butyl 5-(5-chloro-2-cyclopropoxyphenyl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-4-ylcarbamate were dissolved in 50 mL of MeOH. 50 mL of 4 M HCl/MeOH was added dropwise. The mixture was stirred at room temperature overnight. The mixture was evaporated to dryness and purified by silica gel chromatography, eluting with EtOAc to afford 0.25 g of 3-(5-chloro-2-cyclopropoxyphenyl)-1H-pyrazol-4-amine. LCMS (ESI) m+H=249.8. 1H NMR (DMSO-d6, 400 MHz) δ: 12.32-12.10 (br, 1H), 7.41-7.34 (m, 3H), 7.09 (s, 1H), 4.12 (q, J=5.2 Hz, 2H), 2.94-3.88 (m, 3H), 0.79-0.74 (m, 4H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08999998B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-7ac87f60e81041a684e6ce70258f12b0 |
| Source note | uspto-grants-2015_04 |