HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethylamine → HCID 14676164, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethylamine | HCID 1146 | — |
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 14676162 | HCID 14676162 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 14676164 | HCID 14676164 | 60.6% |
Reaction Steps
A mixture of 1-(7-hydroxy-1,2-dihydro-3-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine (0.2 g), ethyl acetate (20 ml), trimethylamine (0.5 g) and benzoyl chloride (0.5 g) is left standing for 7 hours at room temperature. To the mixture is added ethanol (2 ml), and the mixture is left standing overnight. The solvent is distilled off under reduced pressure. To the residue is added ethyl acetate (50 ml), and insolubles are filtered off. The filtrate is concentrated under reduced pressure. The residue is purified by silica gel column chromatography (hexane:acetone=1:1-1:2) and crystallized from ethyl ether to afford 1-(7-benzoyloxy-1,2-dihydro-3-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine (0.15 g) as colorless prisms, m.p. 117°-119° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04880809 |
| Source dataset | uspto-grants-1989_11 |
| ORD ID | ord-50a44acd86844413ac852c11411feb0d |
| Source note | uspto-grants-1989_11 |