HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1,1-dimethylethyl 7-[5-acetyl-2-({[4-(ethyloxy)-2-pyridinyl]methyl}oxy)phenyl]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | 1,1-dimethylethyl 7-(5-acetyl-2-{[(4-chloro-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate | HCID 70664900 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 1,1-dimethylethyl 7-[5-acetyl-2-({[4-(ethyloxy)-2-pyridinyl]methyl}oxy)phenyl]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate | HCID 70665389 | — |
Reaction Steps
Potassium tert-butoxide (0.132 g) in ethanol (4 ml) was stirred for 15 min before adding 1,1-dimethylethyl 7-(5-acetyl-2-{[(4-chloro-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate, (0.4 g) and this was heated in a microwave at 110 C for 1.5 h. Water (20 ml) was added to the cooled mixture and this was extracted with DCM (2×30 ml). The combined organics were washed with brine, dried over sodium sulphate and concentrated in vacuo. The crude product was purified through silica eluting with 0-45% ethyl acetate in hexane to give the title compound, 0.16 g
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08993560B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-d069fd402d9b4d918452211ce1501fa0 |
| Source note | uspto-grants-2015_03 |