HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,2-Trichloroethyl chloroformate → HCID 67252609, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 67253250 | HCID 67253250 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67252609 | HCID 67252609 | 96.3% |
Reaction Steps
To a stirring solution of tert-butyl 7-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)-3,4-dihydroisoquinoline-2(1H)-carboxylate (0.50 g, 1.35 mmol) and Troc-Cl (0.19 ml, 1.38 mmol) in EtOAc (15 mL) was added satd. NaHCO3 (2.75 ml, 2.02 mmol). The resulting biphasic mixture was stirred at RT for 5 h. The layers were separated and the organic washed with sat'd. NaHCO3 (1×) and brine (1×), dried (Na2SO4) and concentrated in vacuo to obtain tert-butyl 7-(3-tert-butyl-5-((2,2,2-trichloroethoxy)carbonyl)-1H-pyrazol-1-yl)-3,4-dihydroisoquinoline-2(1H)-carboxylate (0.69 g, 94% yield). MS (ESI) m/z: 545.0 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07790756B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-6d2963bb6e0145ce8caef528c49d63ac |
| Source note | uspto-grants-2010_09 |