HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 59822300, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 59822286 | HCID 59822286 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59822300 | HCID 59822300 | 94% |
Reaction Steps
Slurry 7-chloro-6-(ethoxycarbonyl)-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (176 g, 503 mmol) and potassium carbonate (348 g, 2516 mmol) in ethanol (1.4 L) and water (1.4 L). Stir the mixture at room temperature for 42 h. Partition the mixture between water (2.6 L) and EtOAc (2.6 L). Collect the organic layer and back extract the aqueous layer with EtOAc (1.8 L). Wash the combined organic extracts successively with water (1.8 L) and brine (1.8 L). Collect the organic layer, dry over Na2SO4 and concentrate in vacuo to obtain the desired intermediate as a green oil (120 g, 94%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994163B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-0b935c31ae114fd6855b6b14762ccd15 |
| Source note | uspto-grants-2011_08 |