HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Acetate → HCID 18378674, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | HCID 54166309 | HCID 54166309 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18378674 | HCID 18378674 | 27.6% |
Reaction Steps
A solution of 8-(4-methylphenylsulfonyl)oxyimino-5,6,7,8-tetrahydroisoquinoline (1.2 g) and potassium acetate (7.45 g) in ethanol (25 ml) and water (30 ml) was heated at 95° C. for 23 hours. The solvent was evaporated at reduced pressure, and the residue was basified with saturated aqueous sodium hydrogencarbonate solution and extracted with chloroform. The dried extract (dried over sodium sulfate) was evaporated at reduced pressure to give crude product. After partial purification by column chromatography (SiO2; 30 g, AcOEt/hexane=2/1, then 5% MeOH—CHCl3), the obtained solid was washed with ether to give 2,3,4,5-tetrahydro-1H-pyrido[3,4-b]azepin-2-one (170 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06495542B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-8fc9e921fc434e1d99a4fd9e30c1d9e0 |
| Source note | uspto-grants-2002_12 |