Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Valeryl chloride | HCID 61186 | — |
| Reactant | 3-Hydrazino-5-methyl-6-phenyl-1,2,4-triazine | HCID 15586409 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 20232065 | HCID 20232065 | 74.6% |
Reaction Steps
A solution of n-valeryl chloride (1.93 g) in methylene chloride (3 ml) was added dropwise to a stirred solution of 3-hydrazino-5-methyl-6-phenyl-1,2,4-triazine (3.224 g) and triethylamine (1.784 g) in methylene chloride (40 ml) under ice cooling, and the stirring was continued for 30 minutes. The reaction mixture was evaporated and the resultant residue was extracted with ethyl acetate after addition of water. The extract was washed successively with 5% hydrochloric acid, water, a saturated aqueous solution of sodium bicarbonate and water, dried over magnesium sulfate, and then concentrated to a small volume under reduced pressure. The resultant residue was crystallized from diethyl ether, collected by filtration, washed with diethyl ether and dried to give 5-methyl-6-phenyl-3-(2-valerylhydrazino)-1,2,4-triazine (3.406 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04616014 |
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| Source dataset | uspto-grants-1986_10 |
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| ORD ID | ord-550a18e95d614adca2c00386aa8c2c24 |
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| Source note | uspto-grants-1986_10 |
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