HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67520922, compound → HCID 67521290, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67520922 | HCID 67520922 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67521290 | HCID 67521290 | 53.8% |
Reaction Steps
A solution of 5,8-dimethoxy-3-[((S)-1-methoxycarbonyl-3-methyl-butylamino)-methyl]-2H-chromene-2-carboxylic acid ethyl ester (3.0 g, 7.12 mmol) and N,N′-diisopropylethyl amine (5.1 mL, 28.5 mmol) in acetonitrile (4 mL) was heated in a sealed tube at 140° C. for 48 h. The reaction mixture, after aqueous work-up, was extracted with ethyl acetate (3×). The combined ethyl acetate layer was washed with brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated in vacuo and the residue was purified over neutral alumina using hexanes-ethyl acetate (1:1.2) as eluents to afford (S)-2-(5,8-dimethoxy-3-oxo-3,9-dihydro-1H-chromeno[2,3-c]pyrrol-2-yl)-4-methyl-pentanoic acid methyl ester (1.4 g, 53.8%) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178689B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-ef3262d3e59a4c7c9d4660343d9b1375 |
| Source note | uspto-grants-2012_05 |