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Oxalyl chloride → 2-(Acetylamino)methyl-5-(3-methoxycarbonylpropionyl)indane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | Mono-Methyl Succinate | HCID 6930703 | — |
| 反応物 | 2-(Acetylaminomethyl)indane | HCID 21476287 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 2-(Acetylamino)methyl-5-(3-methoxycarbonylpropionyl)indane | HCID 21476307 | 93.4% |
反応手順
46.4 g of oxalyl chloride and 2 drops of dimethyl-formamide were added to 48.3 g of monomethyl succinate dissolved in 840 ml of dichloroethane. The mixture was stirred at room temperature for 5 hours. Then, under ice cooling, 34.6 g of 2-(acetylaminomethyl)indane dissolved in 280 ml of dichloroethane and 97.6 g of anhydrous aluminum chloride were added to the reaction mixture. After the mixture was stirred for 1 hour, the reaction mixture was poured into ice water. After the organic layer was collected by separation, washed with water and dried, the solvent was removed to obtain 51.8 g of 2-(acetylaminomethyl)-5-(3-methoxycarbonylpropionyl)indane. m.p.: 139° to 140° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05686452 |
| 出典データセット | uspto-grants-1997_11 |
| ORD ID | ord-9b1b1f762b41442cbb2ff312c4701767 |
| 出典メモ | uspto-grants-1997_11 |