HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67085220, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 67085359 | HCID 67085359 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 67085220 | HCID 67085220 | — |
Reaction Steps
The product of step D was subjected to Boc-deprotection with 2 N HCl in diethyl ether following the procedure of Example 28, step B. The crude material was purified by flash column chromatography (90:9:1 dichloromethane/methanol/ammonium hydroxide) to give 2-phenylsulfonyl-4-fluoro-5-methyl-5,6,7,8,9,10-hexahydro-7,10-epiminocyclohepta[b]indole hydrochloride (40 mg, 84%, HPLC, AUC 97.8%.) as a white solid: mp 251-256° C. dec; 1H NMR (DMSO-d6, 300 MHz): δ 8.24 (d, J=1.5 Hz, 1H), 7.94-8.00 (m, 2H), 7.56-7.70 (m, 3H), 7.48 (dd, J=12.0, 1.5 Hz, 1H), 5.36 (d, J=3.9 Hz, 1H), 4.44-4.52 (m, 1H), 3.82 (s, 3H), 3.34-3.39 (m, 1H), 3.00 (d, J=17.1 Hz, 1H), 2.18-2.30 (m, 2H), 2.03-2.12 (m, 1H), 1.70-1.87 (m, 1H); APCI MS m/z 371 [M+H]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575186B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-60dc074f05d647daab7f71c65a047ce5 |
| Source note | uspto-grants-2013_11 |