HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Oxo-2,3,4,4a, 5,6,8,9-octahydro-1,2,7-triaza-benzocycloheptene-7-carboxylic acid tert-butyl ester → tert-Butyl 3-oxo-2,3,5,6,8,9-hexahydro-7H-pyridazino[3,4-d]azepine-7-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Oxo-2,3,4,4a, 5,6,8,9-octahydro-1,2,7-triaza-benzocycloheptene-7-carboxylic acid tert-butyl ester | HCID 86686512 | — |
| Catalyst | HCID 178418406 | HCID 178418406 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | tert-Butyl 3-oxo-2,3,5,6,8,9-hexahydro-7H-pyridazino[3,4-d]azepine-7-carboxylate | HCID 86686513 | 79.2% |
Reaction Steps
7 g 3-oxo-2,3,4,4a, 5,6,8,9-octahydro-1,2,7-triaza-benzocycloheptene-7-carboxylic acid tert-butyl ester was dissolved in 70 mL toluene and 6.7 g manganese dioxide was added to the reaction mixture. It was heated at reflux for 48 h. After completion of the reaction, the reaction mixture was diluted with chloroform and filtered through celite. The filtrate was concentrated and purified by column chromatography to afford 5.5 g of the desired product. (M+H)+=266
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08642774B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-b4b091f182684dce8868f11e52bdc5ef |
| Source note | uspto-grants-2014_02 |