HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 67071625, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 67071624 | HCID 67071624 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67071625 | HCID 67071625 | 98.4% |
Reaction Steps
A suspension of (±)-(E)-3-[4-oxo-spiro(chromane-2,4′-azepane)-6-yl]acrylic acid methyl ester hydrochloride salt (500 mg, 1.43 mmol, Intermediate 3) in DCM (15 ml) was treated with acetyl chloride (0.121 ml, 1.72 mmol) and DIPEA (0.507 ml, 2.86 mmol) and was stirred at RT for 1. The solution was evaporated under vacuum and the crude product was purified by chromatography column (eluent: DCM/MeOH 95:5) to give (±)-(E)-3-[1′-acetyl-4-oxo-spiro(chromane-2,4′-azepane)-6-yl]-acrylic acid methyl ester (503 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08980877B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-3ca56ae444fa41b1b648a2c2356f649c |
| Source note | uspto-grants-2015_03 |