HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 19841180, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl cyanophosphonate | HCID 76257 | — |
| Reactant | HCID 10106052 | HCID 10106052 | — |
| Reactant | 1-[(3,4,5-Trimethoxyphenyl)methyl]piperazine;dihydrochloride | HCID 12828501 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 19841180 | HCID 19841180 | 27.9% |
Reaction Steps
Using 2,3-dimethoxy-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid (2 g), 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (3.5 g), N,N-dimethylformamide (30 ml), triethylamine (3.3 g) and diethyl phosphorocyanidate (2.5 ml), a reaction as that described in Example 6 is carried out. The product is purified by silica gel column chromatography (hexane:acetone=1:1) to give an oily product which is converted to the hydrochloride in ethyl acetate to yield 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride (1.2 g) as colorless crystals, m.p. 138°-142° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04880809 |
| Source dataset | uspto-grants-1989_11 |
| ORD ID | ord-5738d7cc0dd6438aae278cd6b2cea450 |
| Source note | uspto-grants-1989_11 |