HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68445055, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86628361 | HCID 86628361 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68445055 | HCID 68445055 | 98% |
Reaction Steps
A solution of 1,1-dimethylethyl {1-[(7-fluoro-3-oxo-5,6-dihydro-3H-pyrrolo[1,2,3-de]quinoxalin-6-yl)methyl]-4-piperidinyl}carbamate (8.13 g, 20.2 mmol) in dichloromethane (150 ml) and methanol (100 ml) was cooled in iced water. Hydrogen chloride in 1,4-dioxane (4M, 160 ml) was added gradually, then the mixture was stirred for 1.5 h. The mixture was evaporated and the residue was triturated with ether and filtered off. The solid was partially dissolved in 25% methanol/dichloromethane (200 ml) and stirred with MP-carbonate (3.03 mmol/g, 27 g) for 1 h. The resin was filtered off, washed a few times with 10% methanol/dichloromethane and methanol alternately, and the filtrate was evaporated to give the product (5.96 g, 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07709483B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-d9413c2dc2be4be0b44d57d2f69da04b |
| Source note | uspto-grants-2010_05 |