HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid methylene chloride → (3S,7S)-3-amino-1-methyl-7-phenyl-1,3,4,7-tetrahydro-2H-azepin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | tert-butyl[(3S,7S)-1-methyl-2-oxo-7-phenyl-2,3,4,7-tetrahydro-1H-azepin-3-yl]carbamate | HCID 58691177 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | (3S,7S)-3-amino-1-methyl-7-phenyl-1,3,4,7-tetrahydro-2H-azepin-2-one | HCID 10242432 | 93.6% |
Reaction Steps
To the tert-butyl[(3S,7S)-1-methyl-2-oxo-7-phenyl-2,3,4,7-tetrahydro-1H-azepin-3-yl]carbamate (1d) (200 mg) was added a 1:3 mixture of TFA/DCM (2 ml). The reaction mixture was stirred for 1 h, then diluted with DCM and saturated aq. NaHCO3. The organic layer was isolated and washed with saturated aq. NaHCO3, brine, dried (Na2SO4) and concentrated to yield an oil (128 mg, 93%). MS APCI, m/z=217 (M+1). LC/MS 1.55 min., Method A.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07342007B2 |
| Source dataset | uspto-grants-2008_03 |
| ORD ID | ord-851c11cc1eb74697a3797978b990c0b5 |
| Source note | uspto-grants-2008_03 |