HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18184522, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 18184510 | HCID 18184510 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 18184522 | HCID 18184522 | — |
Reaction Steps
A solution of N-[6-benzyloxy-1-(3,5-dibromo-4-methoxy-benzyl)-1,2,3,4-tetrahydroisoquinolin-7-yl]-methanesulfonamide oxalate (3.98 g, 0.0057 mol) in a mixture of conc. HCl (50 mL) and methanol (50 mL) was refluxed for 1h, cooled and concentrated. A residue was crystallized from methanol—ethyl ether mixture. Yield 2.75 g (87%), M.p. 244-245° C. (dec.). 1H NMR (300 MHz, DMSO) δ 2.9 (s, 3H), 2.95-3.22 (m, 4H), 3.25-3.45 (m, 2H), 3.79 (s, 3H), 4.67 (m, 1H), 6.75 (s, 1H), 7.15 (s, 1H), 7.79 (s, 2H), 8.84 (s, 1H), 9.26 (d, J=12.6 Hz, 2H), 10.18 (s, 1H). Anal. (C18H21Br2ClN2O4S) calcd., C 38.83, H 3.80, N 5.03; found C 38.91, N 4.83.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06596734B1 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-6fc011ac48ad4e8da8c3a45b3e8241e7 |
| Source note | uspto-grants-2003_07 |