HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 66925170, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | HCID 66924919 | HCID 66924919 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66925170 | HCID 66925170 | 50% |
Reaction Steps
2-[(4-{[(tert-Butoxycarbonyl)(methyl)amino]methyl}-2-phenyl-1H-pyrrol-1-yl)sulfonyl]benzoic acid (256 mg) was dissolved in ethyl acetate (1 mL), and 4 mol/L hydrogen chloride-ethyl acetate solution (1 mL) was added at room temperature. After stirring at the same temperature for 3 hr, the reaction mixture was homogenized with methanol, activated carbon was added and the mixture was filtered through celite. The filtrate was concentrated under reduced pressure, and the residue was crystallized from ethyl acetate. The obtained crystal was recrystallized from a mixed solvent of ethyl acetate and ethanol to give the title compound as colorless crystals (yield 110 mg, 50%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08048909B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-31b56f10883a48cfb3c9d725233d7a95 |
| Source note | uspto-grants-2011_11 |