Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 20352656 | HCID 20352656 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 20352652 | HCID 20352652 | 90% |
Reaction Steps
12.4 g of 1-diphenylmethyl-3-methyl-3-(3,4-ethylenedioxybenzyl)-piperazine (3a) are dissolved in 100 ml of dry benzene and combined with 3.3 g of triethylamine. 3.6 g of chloroformic acid ethyl ester in 20 ml of benzene are added dropwise with stirring at room temperature. After 12 hours the solution is washed free of halogen with water and evaporated to dryness in vacuum. 13.1 g (90%) of 1-diphenylmethyl-3-methyl-3-(3,4-ethylenedioxybenzyl)-4-carbethoxypiperazine are obtained (m.p. = 153° - 155° C., diisopropylether), which are dissolved in 100 ml of dry tetrahydrofuran and added dropwise with stirring over 30 minutes to a boiling suspension of 3.8 g of lithium aluminum hydride in 200 ml of tetrahydrofuran. After three hours, the mixture is combined with water and filtered. The filtrate is evaporated to dryness in vacuum. 10.7 g (93%) of 1-diphenylmethyl-3-methyl-3-(3,4-ethylenedioxybenzyl)-4-methylpiperazine are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04088763 |
|---|
| Source dataset | uspto-grants-1978_05 |
|---|
| ORD ID | ord-7dc6176fe4a14b8aa00bdeeb6ea6461e |
|---|
| Source note | uspto-grants-1978_05 |
|---|