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Hydroxyammonium hydrochloride → HCID 178513274、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyammonium hydrochloride | HCID 22029257 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 1-[(6-Chloro-3-pyridyl)methyl]-3-(4-cyanophenyl)-4-oxo-pyrido[1,2-a]pyrimidin-1-ium-2-olate | HCID 86709265 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | HCID 178513274 | HCID 178513274 | — |
反応手順
30 mg (0.08 mmol) of 1-[(6-chloro-3-pyridyl)methyl]-3-(4-cyanophenyl)-4-oxo-pyrido[1,2-a]pyrimidin-1-ium-2-olate (product of step 1) were dissolved in 2 ml DMSO. 13 mg (0.2 mmol) hydroxylammonium hydrochloride and 22 mg (0.2 mmol) potassium t-butoxide were added and the mixture was stirred at room temperature for 18 hours. The mixture was taken up with 10 ml of brine and extracted with ethyl acetate. The organic phases were dried with magnesium chloride and the solvent was removed under reduced pressure. The desired product was sufficiently pure without further purification (10 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09179680B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-19999677997c4cac96f8ae74ea9116a4 |
| 出典メモ | uspto-grants-2015_11 |