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Dimethylformamide diethylacetal → N'-[3-(morpholin-4-yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide diethylacetal | HCID 70913 | — |
| 反応物 | 5-amino-3-(morpholin-4-yl)-1H-pyrazole-4-carbonitrile | HCID 4962657 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N'-[3-(morpholin-4-yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine | HCID 54020168 | — |
反応手順
Under a nitrogen atmosphere, a suspension of 4.00 g (20.7 mmol) of 5-amino-3-(morpholin-4-yl)-1H-pyrazole-4-carbonitrile in 85 ml of toluene is boiled under reflux for 5 hours with 4.17 ml (97%; 23.6 mmol) of N,N-dimethylformamide diethyl acetal, during which the solid dissolves. Cooling to RT (→crystallization), filtration with suction an d washing with toluene and hexane yield N′-[3-(morpholin-4-yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine; m.p. 182-183° C.; TLC: Rf=0.20 (ethyl acetate).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06251911B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-2267d8654dfb42d1ab8ac664cd0cce9e |
| 出典メモ | uspto-grants-2001_06 |