関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Tin tetrachloride | HCID 24287 | — |
| 反応物 | 2-(1H-Pyrrol-1-yl)isoindoline-1,3-dione | HCID 853719 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(2-Acetyl-1H-pyrrol-1-yl)-1H-isoindole-1,3(2H)dione | HCID 19966752 | — |
反応手順
To a stirred solution of acetyl chloride (6.77 ml) in DCM (400 ml) was added tin (IV) chloride (11.14 ml) at -5° C., under nitrogen. 2-(1H-pyrrol-1-yl)-1H-isoindole-1,3(2H)dione (20.0 g) was then added portion-wise, keeping the temperature below 0° C. The reaction mixture was then stirred at 0° C. for 0.5 hour, at which time it was poured into ice water. The layers were separated and the aqueous phase was extracted with DCM. The combined organics were washed twice with 5% HCl (aq.) and dried (MgSO4). Filtration and concentration gave the crude product. Purification via flash column chromatography (silica gel, DCM) afforded 9.62 g of the product as a solid, m.p. 204°-205° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05274116 |
|---|
| 出典データセット | uspto-grants-1993_12 |
|---|
| ORD ID | ord-f93122ad51fa457cad3eb1429ab1d2f6 |
|---|
| 出典メモ | uspto-grants-1993_12 |
|---|