Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trityl chloride | HCID 6456 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Piperazineethanol | HCID 91308 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19004143 | HCID 19004143 | 33.3% |
Reaction Steps
To a mixture of 255 mg (1.96 mmol) of (±) 2-(2-hydroxyethyl)piperazine and 1.25 g (4.50 mmol) of triphenylmethyl chloride in 5.0 ml of methylene chloride was added 550 ml (3.95 mmol) of triethylamine in one portion and the mixture was stirred at room temperature overnight under a nitrogen atmosphere. The reaction was diluted with 5 mL of methylene chloride and washed with water (3×5 ml) and the layers separated. The aqueous layer was extracted with 10 mL of methylene chloride. The organic layers were combined and washed with 15 mL of saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to an orange foam. Flash chromatography on 75 g of silica gel using a gradient elution of 1:9 v/v ethyl acetate/hexane to 1:9 v/v ethanol/ethyl acetate yielded 401 mg (33%) of a foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05344830 |
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| Source dataset | uspto-grants-1994_09 |
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| ORD ID | ord-4b3a227fe2f740118f4861dd8b81ac7c |
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| Source note | uspto-grants-1994_09 |
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