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Phthaloyl chloride → 2-Bromo-4,5-dimethoxyl-(2-phthalimidoethyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phthaloyl chloride | HCID 6955 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Br-4,5-DMPEA | HCID 820370 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Bromo-4,5-dimethoxyl-(2-phthalimidoethyl)benzene | HCID 5061742 | — |
反応手順
2-Bromo-4,5-dimethoxylbenzeneethanamine (3.5 g 13.2 mmol) was dissolved and stirred in 50 mL dry acetonitrile. 2.14 mL (1.1 equiv) phthaloyl dichloride and 7 mL (3 equiv) Hünig's base were added. The mixture was stirred at room temperature overnight. Acetonitrile was then removed, and the remaining product was taken up in dichloromethane and washed with basic water (pH=11). The aqueous wash was extracted with dichloromethane 3×15 mL. The organic fractions were combined and dried over sodium sulfate. Solvent was removed to give the crude product, which was then purified by column chromatography. Calculated yield: 1.8 g (34%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09302990B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-cc7969ff3c2a4c9bbd52b66808ab44a1 |
| 出典メモ | uspto-grants-2016_04 |