化工社化工社 化学情報印刷レポート · 研究参考用
Water → N-methyl-benzimidic acid 1,3-dioxo-1,3-dihydro-isoindol-2-yl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | N-Methylbenzimidoyl chloride | HCID 576277 | — |
| 反応物 | n-Hydroxyphthalimide sodium salt | HCID 67549515 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-methyl-benzimidic acid 1,3-dioxo-1,3-dihydro-isoindol-2-yl ester | HCID 59305847 | — |
反応手順
N-hydroxy phthalimide sodium salt (46.25 g.; 0.25 mol), is dissolved in dry DMF (220 ml), to the resulting suspension 38.8 g (0.25 mol) of N-methyl benzimidoyl chloride (prepared according to J. C. S. Perkin II, 1324, (1980)) are slowly added at room temperature, on stirring. The reaction mixture is stirred at room temperature for 19 h and then poured into 1.5 l of water. The so formed precipitate is sucked off and dried in vacuo to obtain 66.06 g of a a crude product which is then taken up in 250 ml of acetonitrile. After filtration 58.7 g of N-methyl-benzimidic acid 1,3-dioxo-1,3-dihydro-isoindol-2-yl ester are obtained in form of colorless crystals, mp. 174-176° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07723399B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-5f0a33363701454c8f911a2ac82d2d4a |
| 出典メモ | uspto-grants-2010_05 |