Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 135444679 | HCID 135444679 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 135423037 | HCID 135423037 | 48.3% |
Reaction Steps
384 mg (0.988 mmol) of 5-(hydroxy-phenyl-methyl)-3-(1-methyl-4-phenyl-butyl)-3,6-dihydro-[1,2,3]triazolo[4,5-d]pyrimidin-7-one are dissolved in a mixture of 3 ml of DMSO and 10 ml of dichloromethane, and the solution is cooled to 0° C. 1.37 ml (9.88 mmol) of triethylamine and 692 mg (4.35 mmol) of pyridine-SO3 complex are added, and the reaction mixture is then stirred at room temperature for 15 hours. For work-up, the mixture is diluted with 100 ml of dichloromethane and the organic phase is washed with 1N HCl and saturated sodium bicarbonate solution and then dried over sodium sulphate. The solvent is removed, and chromatographic purification gives 185 mg (48%) of a solid, m.p.: 105° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06458796B1 |
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| Source dataset | uspto-grants-2002_10 |
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| ORD ID | ord-1eda5685f32a4224a877b587e88466c3 |
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| Source note | uspto-grants-2002_10 |
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