HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67085227, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 57392614 | HCID 57392614 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67085227 | HCID 67085227 | — |
Reaction Steps
To a solution of product from step B (25 mg, 0.07 mmol) in methanol (0.5 mL) and dichloromethane (0.5 mL) was added 1.25 M HCl in methanol (0.22 mL). The solution was concentrated in vacuo and the residue lyophilized to give 2-(3-thienyl)sulfonyl-5-methyl-5,6,7,8,9,10-hexahydro-7,10-epiminocyclohepta[b]indole hydrochloride (26 mg, 94%; AUC HPLC 98.5%) as a white solid. mp 208-212° C. dec; 1H NMR (DMSO-d6, 300 MHz) δ 9.56 (br s, 1H), 9.30 (br s, 1H), 8.30-8.39 (m, 2H), 7.63-7.76 (m, 3H), 7.39 (dd, J=5.1, 1.5 Hz, 1H), 5.31-5.39 (m, 1H), 4.42-4.52 (m, 1H), 3.68 (s, 3H), 3.31-3.44 (m, 1H), 3.01 (d, J=17.4 Hz, 1H), 2.20-2.36 (m, 2H), 2.01-2.14 (m, 1H), 1.72-1.89 (m, 1H); ESI, m/z 359 [M+H]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575186B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-f7f73069817b400fad0e039c5e18e232 |
| Source note | uspto-grants-2013_11 |