HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 53942559, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Dibenzo(c,f)pyrazino(1,2-a)azepine, 1,2,3,4,10,14b-hexahydro-2-methyl-, (14bS)- | HCID 154315 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 53942559 | HCID 53942559 | 98% |
Reaction Steps
A solution of 5.52 g of (S)-1,2,3.4,10,14b-hexahydro-2-methyldibenzo[c,f]pyrazino[1,2-a]azepine (prepared as described in preparation 6) in 30 ml of toluene was added dropwise to a solution of 6.8 g of ethyl chloroformate in 50 ml of toluene at 80° C. over a period of 10 minutes, and the mixture was heated under reflux for 3 hours. At the end of this time, the crystals which precipitated were removed by filtration, and solvent was removed from the filtrate by evaporation under reduced pressure, to give 6.57 g (yield 98%) of the title compound as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05476848 |
| Source dataset | uspto-grants-1995_12 |
| ORD ID | ord-7696a1471f5a449693f22e4edb31aeb6 |
| Source note | uspto-grants-1995_12 |