関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(4-Pyridylmethyl)-1(2H)-phtalazinone | HCID 789954 | — |
| 反応物 | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
反応手順
Under exclusion of air, 29 g (122 mmol) 4-(4-pyridylmethyl)-1(2H)-phthalazinone [for preparation, see German Auslegeschrift no. 1061788 (published Jul. 23, 1959)] in 450 ml acetonitrile is mixed with 61 ml HCl/dioxane 4N and 28 ml (306 mmol) phosphoryl chloride and stirred for 27 h at 50° C. To the white suspension, 119 g NaHCO3 in 1.45 l water is then added dropwise under ice cooling, and the mixture is stirred and the title compound filtered off. Anal. calc.(C14H10N3Cl) C, 65.76%; H, 3.94%; N, 16.43%, Cl, 13.86%. found C, 65.40%; H, 4.12%; N, 16.45%, Cl, 13.66%; FAB MS (M+H)+=256
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06710047B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-01521d7212634deb946f50a304f146de |
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| 出典メモ | uspto-grants-2004_03 |
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