HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-[4-(p-Chlorbenzylamino)-6-Methyl-2-Pyrimidinylthio]Acetamidoxime
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | [4-(p-Chlorobenzylamino)-6-methyl-2-Pyrimidinylthio]Acetonitrile | HCID 12228967 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-[4-(p-Chlorbenzylamino)-6-Methyl-2-Pyrimidinylthio]Acetamidoxime | HCID 54511950 | — |
Reaction Steps
A mixture of 10.6g. (0.035 mole) of [4-(p-chlorobenzylamino)-6-methyl-2-pyrimidinylthio]acetonitrile, 4.83 g. (0.07 mole) of hydroxylamine hydrochloride and 14.7 g. (0.14 mole) of sodium carbonate in 100 ml of N,N-dimethylformamide was heated on a steam bath for 3 hours. The mixture was filtered and the filtrate evaporated in a rotary-evaporator. The residue was triturated with petroleum ether containing a little ethyl acetate. The solid which crystallized was collected and recrystallized from ethyl acetate to give pure free base, m.p. 113°-116°. This free base was dissolved in absolute ethanol and acidified with an ethereal hydrochloric acid solution to give 3.5 g. of product, as the dihydrochloric salt, m.p. 230°-232° d.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03950339 |
| Source dataset | uspto-grants-1976_04 |
| ORD ID | ord-abdb051e69f74fad84db5afa1229849c |
| Source note | uspto-grants-1976_04 |