HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl N-(triethylammoniosulfonyl)carbamate → HCID 71293436, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl N-(triethylammoniosulfonyl)carbamate | HCID 2724994 | — |
| Reactant | HCID 71293427 | HCID 71293427 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71293436 | HCID 71293436 | 38.5% |
Reaction Steps
Intermediate 13 (92 mg, 0.209 mmol) was dissolved in THF (8 mL), and Burgess reagent (150 mg, 0.63 mmol) was added. The reaction mixture was stirred at RT for 30 mins and was then partitioned between EtOAc and water. The organic layer was separated, and the aqueous layer further extracted with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4) and evaporated in vacuo. The resulting residue was purified by silica gel chromatography eluting with 80% EtOAc in cyclohexane as eluent to yield a white solid. Further purification was carried out by reverse phase HPLC using a gradient of 40-98% MeCN in water (+0.1% formic acid) to yield the title compound as a white solid (34 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08691826B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-884163f011884674b57c23c02f44b96f |
| Source note | uspto-grants-2014_04 |