HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-(4-Methoxyphenyl)-4-[2-(1,3,4,5-tetrahydrobenzo[c]oxepin-1-yl)-ethyl]-piperazine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | p-Methoxyphenylpiperazine | HCID 23170892 | — |
| Reactant | 1-(4-Methoxyphenyl)-4-(1,3,4,5-tetrahydrobenzo[c]oxepin-1-yl)acetyl piperazine | HCID 23288865 | — |
| Reactant | HCID 23288902 | HCID 23288902 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 1-(4-Methoxyphenyl)-4-[2-(1,3,4,5-tetrahydrobenzo[c]oxepin-1-yl)-ethyl]-piperazine hydrochloride | HCID 23288845 | — |
Reaction Steps
Step 5--Following the general procedure of EXAMPLE 50 and making non-critical variations p-methoxyphenylpiperazine is acylated with (1,3,4,5-tetrahydrobenzo[c]oxepin-1-yl)acetic acid (CXXIII, 619 mg) and the resulting amide, 1-(4-methoxyphenyl)-4-(1,3,4,5-tetrahydrobenzo[c]oxepin-1-yl)acetyl piperazine (CXXIV, 1.07 g) is reduced according to the general procedure described in EXAMPLE 50 (making non-critical variations) to give crude product. This crude material is dissolved in ether (30 ml) and methanol (3 ml) and treated with gaseous hydrochloric acid resulting in the formation of a salt. This crude salt is recrystallized from methanol/ethyl acetate to give the title compound, mp 217.0-219.0° (uncorrected, decomp).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06133446 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-4ac523aa53e84a35bf6200d449e4df7d |
| Source note | uspto-grants-2000_10 |