HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 18184534, compound → HCID 18184532, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 18184534 | HCID 18184534 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 18184532 | HCID 18184532 | — |
Reaction Steps
A solution of N-[6-benzyloxy-1-(3,4-dichloro-benzyl)-1,2,3,4-tetrahydro-isoquinolin-7-yl]-methanesulfonamide oxalate (0.5 g, 0.00085 mol) in 15 mL of acetic acid and 30 mL of conc. HCl was refluxed for 1 h, evaporated to dryness and the residue was crystallized from methanol-ether mixture. Yield 0.23 g (62%). mp 249-250° C. 1H NMR (Me2SO-d6) 300 MHz: δ 10.17 (s, 1H), 9.23 (brs, 2H), 8.84 (s, 1H), 7.75 (s, 1H), 7.61 (d, J=7.8 Hz, 1H), 7.42 (d, J=8.1 Hz, 1H), 7.10 (s, 1H), 6.75 (s, 1H), 4.70 (brs, 1H), 3.28-3.43 (brs, 4H), 3.10-3.22 (m, 1H), 2.96-3.04 (m, 1H), 2.90 (s, 3H). MS (ESI): 402 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06596734B1 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-4115a39d5a574994951cc791db4fa452 |
| Source note | uspto-grants-2003_07 |