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Sodium Carbonate → 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Chloride dihydrate | HCID 21226388 | — |
| 反応物 | 1-(2-Nitrophenyl)-2-pyrroleacetic acid, ethyl ester | HCID 86183131 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one | HCID 12359340 | 100.9% |
反応手順
To a solution of 0.8 mmol of 1-(2-nitrophenyl)-2-pyrroleacetic acid, ethyl ester in 3 ml of ethanol is added stannus chloride dihydrate (SnCl2. 2H2O) in 2 ml of concentrated hydrochloric acid (with cooling in water bath). The mixture is stirred at room temperature for 5 hours and chilled in an ice bath. To the mixture is added slowly saturated sodium carbonate solution. The solid which precipitates is filtered and the solid washed with water and then extracted with ethyl acetate. The ethyl acetate extract is dried (Na2SO4) and the solvent removed to give 0.16 g of solid which is triturated with ether to give 0.11 g of product as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624923 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-c57882da43454c61b636c60b0b206209 |
| 出典メモ | uspto-grants-1997_04 |