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Hydrochloric Acid → 5,5-dimethyl-3-[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]imidazolidine-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | methyl 2-methyl-2-[[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]carbamoylamino]propanoate | HCID 57786643 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5,5-dimethyl-3-[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]imidazolidine-2,4-dione | HCID 25221266 | — |
反応手順
To a solution of methyl 2-methyl-2-[[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]carbamoylamino]propanoate (14) (44 mg, 0.11 mmol) in dry DMF (2 mL) was added finely powdered sodium hydroxide (4 mg, 0.072 mmol). The reaction mixture was immersed in a preheated oil bath at 50° C. for 5 hours, before being neutralized by addition of 1M HCl The desired product was isolated from the resultant solution by preparative chromatography to yield a solid (3.6 mg, 98% purity). M/z (LC-MS, ESP), RT=7.69 mins (M+H 367.1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07981890B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-c485a3fa48f245b0abdaf29b7fbf93f5 |
| 出典メモ | uspto-grants-2011_07 |