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Phthalic Anhydride → 2-(Dimethylamino)isoindoline-1,3-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phthalic Anhydride | HCID 6811 | — |
| 反応物 | N,N-Diethylaniline | HCID 7061 | — |
| 反応物 | 1,1-Dimethylhydrazine dihydrochloride | HCID 3016972 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(Dimethylamino)isoindoline-1,3-dione | HCID 248976 | 85% |
反応手順
To the suspension of phthalic anhydride (62.5 mmol) in toluene (500 ml), N,N-dimethyl hydrazine dihydrochloride (50 mmol) and diethyl-phenyl-amine (90 mmol) were added. The reaction mixture was refluxed for 18 hours while removing the formed water via a Dean-Stark trap. Then, toluene was evaporated under reduced pressure and the resulting crude was purified on silica gel chromatography with (1:5) EtOAc:dichloromethane, to give the desired product in 85% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541428B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-9556816542c64a74867182946ad62c50 |
| 出典メモ | uspto-grants-2013_09 |