HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → (+/-)-2-Methyl-3-amino-N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-N-isobutylpropanamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | (+/-)-2-Methyl-3-(methylpropan-2-yl)oxycarbonylamino-N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-N-isobutylpropanamide | HCID 66726391 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (+/-)-2-Methyl-3-amino-N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-N-isobutylpropanamide | HCID 58080637 | — |
Reaction Steps
The above (±)-2-Methyl-3-(methylpropan-2-yl)oxycarbonylamino-N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-N-isobutylpropanamide was dissolved in dichloromethane (3 ml) and treated with trifluoroacetic acid (3 ml). After stirring for two hours at room temperature, the reaction mixture was concentrated under reduced pressure. The residue was partitioned between dichloromethane (10 mL) and aq. sodium carbonate (sat., 10 mL). The aqueous layer was extracted with dichloromethane (10 ml×2). After washing with brine, the organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure to yield a resin: MS (m+1)=355.5.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722896B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-b2f66c3ba5e1408ebe51e301b6913130 |
| Source note | uspto-grants-2014_05 |