Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 54370034 | HCID 54370034 | — |
| Product | HCID 15382032 | HCID 15382032 | — |
Reaction Steps
A solution of 1.000 g of 1-(3-phenylcinnamoyl)-4-[3,4,5-trimethoxy(thiobenzoyl)]piperazine (prepared as described in Example 61) in 10 ml of benzene and 0.805 g of Lawesson's Reagent [consisting mainly of [2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide] was heated under reflux for 2 hours. At the end of this time, the reaction mixture was cooled to room temperature, poured into water and extracted twice with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate, and concentrated by distillation under reduced pressure. The residue was purified by column chromatography through 30 g of silica gel eluted with a 3:1 by volume mixture of hexane and ethyl acetate, to give 1.010 g of the title compound as a yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05369106 |
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| Source dataset | uspto-grants-1994_11 |
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| ORD ID | ord-706743a62c5a4209a98baeb64f8a674c |
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| Source note | uspto-grants-1994_11 |
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