Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 1-Phenethylamine, (+)- | HCID 643189 | — |
| Reactant | HCID 22466443 | HCID 22466443 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 53830131 | HCID 53830131 | 77% |
Reaction Steps
Reaction under N2 atmosphere. Na2CO3 (0.01 mol) was added to a mixture of 2-(2-bromoethyl)-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-3H -1,2,4-triazol-3-one (0.0054 mol) in 1-methyl-2-pyrrolidinone (25 ml). This mixture was stirred at 60° C. A solution of (+)-(R)-α-methylbenzenemethanamine (0.0065 mol) in 1-methyl-2-pyrrolidinone (25 ml) was added dropwise and the resulting reaction mixture was stirred overnight at 60° C. The reaction mixture was cooled, poured out into ice-water and the resulting precipitate was filtered off, washed with water, then dried. This fraction was recrystallized from 2-propanol, filtered off and dried, yielding 1.98 g (77%)of (R)-2,4-dihydro4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-2-[2-[(1-phenylethyl)amino]ethyl]-3H-1,2,4-Triazol-3-one (interm. 19).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06384030B1 |
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| Source dataset | uspto-grants-2002_05 |
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| ORD ID | ord-38eb8d43612e4f8ebbfe126c8d459654 |
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| Source note | uspto-grants-2002_05 |
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