HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67085143, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 67173431 | HCID 67173431 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 67085143 | HCID 67085143 | — |
Reaction Steps
To a solution of the product of step D (70 mg, 0.13 mmol) in methanol was added 2M HCl in diethylether (4 mL). After stirring for 2 h, the solution was concentrated in vacuo, triturated with ethyl acetate, and lyophilized from water to give 2-phenylsulfonyl-5-phenyl-5,6,7,8,9,10-hexahydro-7,10-epiminocyclohepta[b]indole hydrochloride (50 mg, 57%, AUC HPLC >99%) as a white solid: mp 195-200° C.; 1H NMR (CD3OD, 300 MHz) δ 8.38 (d, J=1.8 Hz, 1H), 7.95-7.99 (m, 2H), 7.72 (dd, J=8.8, 1.5 Hz, 1H), 7.51-7.64 (m, 6H), 7.39-7.42 (m, 2H), 7.32 (d, J=9.0 Hz, 1H), 5.39-5.40 (m, 1H), 4.49 (br s, 1H), 3.39 (dd, J=8.7, 4.5 Hz, 1H), 2.81 (d, J=17.7 Hz, 1H), 2.37-2.46 (m, 3H), 1.98-2.08 (m, 1H); ESI, m/z 415 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575186B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-ed8a1cf9b6674a49b1a194b38df2a622 |
| Source note | uspto-grants-2013_11 |