HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-Allyl-7-bromo-2,3-dihydro-1-benzazepine-4-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Allyl 1-allyl-7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate | HCID 22329223 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Allyl-7-bromo-2,3-dihydro-1-benzazepine-4-carboxylic acid | HCID 22329279 | 99.9% |
Reaction Steps
To a solution of allyl 1-allyl-7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate (224 mg) in tetrahydrofuran (10 ml) were added tetrakistriphenylphosphinepalladium (74 mg) and morpholine (560 mg), and the mixture was stirred under argon atmosphere at room temperature for 2 hours. To the mixture was added water at 0° C., and the mixture was made acidic (pH=4) with 1N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, further with water and saturated brine and dried with magnesium sulfate. The solvent was evaporated under reduced pressure to give 1-allyl-7-bromo-2,3-dihydro-1-benzazepine-4-carboxylic acid (198 mg) as yellow amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06936602B1 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-228ad3cd8e0d4f48ac1dcb0387cd6386 |
| Source note | uspto-grants-2005_08 |