HuagongsheHuagongshe Chemistry Print Report · For research reference only
ethyl 4-methylene-7,8-dihydro-4H-thieno[2,3-d]azepine-6(5H)-carboxylate → 4-Methyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | ethyl 4-methylene-7,8-dihydro-4H-thieno[2,3-d]azepine-6(5H)-carboxylate | HCID 58293774 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-Methyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester | HCID 59302556 | — |
Reaction Steps
Compound 1030 (310 mg, 1.31 mmol) was dissolved in ethanol (50 mL). The solution was degassed three times before addition of 10% Pd/C (100 mg). The flask was charged with hydrogen at atmospheric pressure (H2 balloon) and stirred at RT for 14 hours. The catalyst was removed by filtration through diatomaceous earth and the volatiles removed under reduced pressure to yield ethyl 4,5,7,8-tetrahydro-4-methylthieno[3,2-d]azepine-6-carboxylate (Compound 1031), which was used in subsequent reactions without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481524B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-90d4f64eb0954a16a562fc473a1adc14 |
| Source note | uspto-grants-2013_07 |