HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178423625, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | (3'S,4'R,7'S,8'S,8a'R)-6''-chloro-8'-(3-chloro-2-fluorophenyl)-4,4-dimethyl-3',4'-diphenyl-3',4',8',8a'-tetrahydro-1'H-dispiro[cyclohexane-1,6'-pyrrolo[2,1-c][1,4]oxazine-7',3''-indole]-1',2''(1''H)-dione | HCID 70872025 | — |
| Reactant | HCID 178511715 | HCID 178511715 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178423625 | HCID 178423625 | 101.1% |
Reaction Steps
Trans-4-aminocyclohexanol (167 mg, 1.45 mmol) was added to a tetrahydrofuran (10 ml) solution of the compound (194 mg, 0.29 mmol) obtained in Step 1 above and the resulting mixture was heated to reflux for 6 days. After cooling, saturated ammonium chloride solution was added, followed by extraction with ethyl acetate. The organic layer was washed with brine and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography [chloroform:methanol=100:0→30:1 (v/v)] to give 230 mg (100%) of the title compound as a pale yellow amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629133B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-cf2c73dae4c74c8380bede9d332945eb |
| Source note | uspto-grants-2014_01 |