HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 19841239, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diethyl cyanophosphonate | HCID 76257 | — |
| Reactant | HCID 10467188 | HCID 10467188 | — |
| Reactant | 1-[(3,4,5-Trimethoxyphenyl)methyl]piperazine;dihydrochloride | HCID 12828501 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19841239 | HCID 19841239 | 42.7% |
Reaction Steps
Using a mixture of 3,4-dimethoxy6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid (0.6 g), 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (1.3 g), triethylamine (1.5 g), N,N-dimethylformamide (20 ml) and diethyl phosphorocyanidate (0.6 ml), an amidation as that described in Example 6 is carried out. The product is purified by silica gel column chromatography (hexane:acetone=1:1), and converted to the hydrochloride in a mixture of ethyl acetate and ethyl ether to yield 1-(3,4-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride (0.55 g) as colorless crystals, m.p. 225°-229° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04880809 |
| Source dataset | uspto-grants-1989_11 |
| ORD ID | ord-a674d7f71535476b86a46f0188a7fdcf |
| Source note | uspto-grants-1989_11 |