HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2,3,4,5-Tetrahydro-1H-1-benzazepine-7,9-di-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Water ethanol | HCID 19096565 | — |
| Reactant | 7-Cyano-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid benzyl ester | HCID 53681205 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2,3,4,5-Tetrahydro-1H-1-benzazepine-7,9-di-carboxylic acid | HCID 19797205 | 85% |
Reaction Steps
7-Cyano-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid benzyl ester (3.30 g) and sodium hydroxide (2 g) in a mixed solution of water-ethanol (1:1, 60 ml) was refluxed for 8 hours. After cooled, water (100 ml) was added to the reaction mixture, which was then rendered to have pH 3 with concentrated hydrochloric acid. The deposited crystal was collected by filtration, washed with water and dried to give the intended compound 1.84 g (85.0%), which was then recrystallized from ethanol to give slightly yellow crystal. M.P.: 287°-288° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05242912 |
| Source dataset | uspto-grants-1993_09 |
| ORD ID | ord-ca2fd54a918b4c22a80531e0a6588ec9 |
| Source note | uspto-grants-1993_09 |