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Methanol → 1,6-Dihydro-5(4H)-pyrimidinone O-methyloxime monohydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | O-methylhydroxylammonium chloride | HCID 11639 | — |
| 反応物 | 1,3-Diaminopropan-2-one--hydrogen chloride--water (1/2/1) | HCID 19083739 | — |
| 生成物 | 1,6-Dihydro-5(4H)-pyrimidinone O-methyloxime monohydrochloride | HCID 73605605 | 36% |
反応手順
1,3-Diaminoacetone dihydrochloride monohydrate (2.61 g, 14.6 mmol) was dissolved in refluxing methanol. To this solution o-methylhydroxylamine hydrochloride (2.43 g, 29.2 mmol) was added. After reflexing for 48 hours the solvents were evaporated. The crude product was dissolved in methanol and an excess of trimethylorthoformate was added to the reaction mixture which was heated to reflux. After 24 hours the solvent was removed in vacuo. crystallization from methanol/ethyl acetate afforded 850 mg (36%) of a light-brown crystalline material. Mp. 170.7° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05470856 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-5a0b5e02eefc472db4304a28baf660fa |
| 出典メモ | uspto-grants-1995_11 |