HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 90066696, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | tert-butyl 2-(5-(methoxycarbonyl)-2,4-dimethylphenyl)-4,5,7,8-tetrahydroimidazo[4,5-d]azepine-6(1H)-carboxylate | HCID 90066697 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 90066696 | HCID 90066696 | — |
Reaction Steps
Into a 100-mL round-bottom flask, was placed a solution of tert-butyl 2-(5-(methoxycarbonyl)-2,4-dimethylphenyl)-4,5,7,8-tetrahydroimidazo[4,5-d]azepine-6(1H)-carboxylate (compound 83.3, 800 mg, 2.00 mmol) in dichloromethane (16 mL). Trifluoroacetic acid (4 mL) was added drop-wise and the resulting solution was stirred for 5 h at room temperature. The pH of the solution was carefully adjusted to 8-9 with NaHCO3 (sat.) and the aqueous phase was extracted with DCM (3×30 mL), and the combined organics were dried (Na2SO4), filtered, and concentrated under reduced pressure to yield 0.60 mg (crude) of the title compound as brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09428502B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-a52fd320088f4b1db8f0621608206865 |
| Source note | uspto-grants-2016_08 |