HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-Formyl-1,2,7,8,9,10,11,13-octahydro-13-oxo-4-(propylthio)-[l]benzothieno[2',3': 4,5] pyrimido[1,2-a]azepine-9-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 59381648 | HCID 59381648 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 3-Formyl-1,2,7,8,9,10,11,13-octahydro-13-oxo-4-(propylthio)-[l]benzothieno[2',3': 4,5] pyrimido[1,2-a]azepine-9-carboxylic acid methyl ester | HCID 59381663 | — |
Reaction Steps
Compound 22 80.37 mmol) was dissolved into MeOH (10 ml), and KOH (0.98 mmol) in MeOH (5 ml) was added. The reaction mixture was stirred for 2 hours in room temperature. The reaction mixture was poured into water, acidified with HCl and extracted with CH2Cl2. Organic layer was washed with brine and dried with Na2SO4. After filtration the solvent was evaporated. Purification by flash chromatography using CH2Cl2-EtOAc 9:1 as an eluent afforded compound 23 as a major product and compound 24 as a minor product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07754709B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-c80509920b2f4c11ba597173c2cdc9bc |
| Source note | uspto-grants-2010_07 |