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Isopropanol → 4-[(3-Chloro-4-methoxybenzyl)amino]-1(4-hydroxypiperidino)-6-phthalazine carbothiamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Diethyldithiophosphate | HCID 53249491 | — |
| 反応物 | 4-[(3-Chloro-4-methoxybenzyl)amino]-1-(hydroxypiperidino)-6-phthalazine carbonitrile | HCID 86588312 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-[(3-Chloro-4-methoxybenzyl)amino]-1(4-hydroxypiperidino)-6-phthalazine carbothiamide | HCID 9933834 | — |
反応手順
3.7 ml diethyl dithiophosphate was added to a mixture of 2.0 g 4-[(3-chloro-4-methoxybenzyl)amino]-1-(hydroxypiperidino)-6-phthalazine carbonitrile, 1 ml water and 2 ml isopropanol, and the mixture was heated under reflux for 1 hr. After cooling, water was added to the reaction solution and the resulting crystals were collected by filtration. The filtrate was extracted with ethyl acetate and washed with brine. It was dried over anhydrous sodium sulfate, and filtered. The filtrate was evaporated, and the resulting crystalline residue was combined with the crystals collected above by filtration, whereby 1.5 g of the title compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699870B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-5695479b783148a5bdc14f2c5cdf229d |
| 出典メモ | uspto-grants-2004_03 |