Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | 2,3-Dimethoxyphenol | HCID 78828 | — |
| Reactant | Methyl piperazine-1-carbodithioate | HCID 21278808 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19388487 | HCID 19388487 | 51.5% |
Reaction Steps
In 10 ml of ethanol was dissolved 0.86 g of 35% formalin. To the solution was dropwise added under chilling with ice a solution of 2.35 g of methyl 1-piperazinecarbodithioate in 5 ml of ethanol. The mixture was then stirred for 30 min. at room temperature. The mixture was refluxed overnight under heating after addition of a solution of 1.54 g of 2,3-dimethoxyphenol in 5 ml of ethanol under chilling with ice. The reaction mixture was cooled to room temperature. The solvent was distilledoff under reduced pressure, and the residue was purified by silica gel column chromatography. The eluate was treated with 10 ml of ethanol to obtain a crystalline product. The product was collected by filtration and washed with ethanol to give 1.76 g of the desired compound as a pale yellow crystalline product, m.p. 113° C. (decomp.), yield 51.5%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05446146 |
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| Source dataset | uspto-grants-1995_08 |
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| ORD ID | ord-2b7925f2a9e1438682681a4b84918dcb |
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| Source note | uspto-grants-1995_08 |
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