HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 67071433, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 67071461 | HCID 67071461 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67071433 | HCID 67071433 | 99.6% |
Reaction Steps
Acetyl chloride (168 mg, 2.14 mmol) was added dropwise to a stirred solution of (±)-(E)-3-[4-oxo-spiro(chromane-2,3′-piperidine)-6-yl]-acrylic acid methyl ester (Intermediate 2, 600 mg, 1.78 mmol) and TEA (0.742 ml, 5.33 mmol) in DCM (30 ml). The resulting mixture was stirred overnight at RT, then washed with 5% NaHCO3, brine and dried over Na2SO4. The crude mixture was purified by column chromatography (eluent: DCM/MeOH 99:1) to give (±)-(E)-3-[1′-acetyl-4-oxo-spiro(chromane-2,3′-piperidine)-6-yl]-acrylic acid methyl ester (609 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08980877B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-ce882998796743d6bb658dd375a7592b |
| Source note | uspto-grants-2015_03 |