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Methanol → 1,6-Dihydro-5(4H)-pyrimidinone O-(cyclopropylmethyl)-oxime monohydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | O-(cyclopropylmethyl)hydroxylamine hydrochloride | HCID 11557279 | — |
| 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-(cyclopropylmethyl)-oxime monohydrochloride | HCID 73605624 | 57% |
反応手順
1,3-Diaminoacetone dihydrochloride monohydrate (2.00 g, 11.2 mmol) was dissolved in refluxing methanol and O-(cyclopropylmethyl)hydroxylamine hydrochloride (2.60 g, 21.1 mmol) was added. After refluxing for 96 hours the solvent was 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 48 hours the solvent was removed in vacuo. Crystallization from methanol/ethyl acetate afforded 1.30 g (57%) of light-brown material. Mp. 158.0° 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-d8f0e0c4d17e451189d6b77c3659d688 |
| 出典メモ | uspto-grants-1995_11 |