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Sodium Carbonate → Pyrrolo(3,2-b)(1,5)benzodiazepin-10(1H)-one, 4,9-dihydro-1,3-dimethyl-4-(1-oxo-3-(1-pyrrolidinyl)propyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 4-(3-Bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one | HCID 20515487 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Pyrrolo(3,2-b)(1,5)benzodiazepin-10(1H)-one, 4,9-dihydro-1,3-dimethyl-4-(1-oxo-3-(1-pyrrolidinyl)propyl)- | HCID 3068589 | — |
反応手順
1.9 g of 4-(3-bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one and 0.75 g of pyrrolidine are warmed at 80° C. for 4 hours in 50 ml of dioxane. After the solvent has been stripped off in vacuo, the residue is taken up in a little saturated sodium carbonate solution. The mixture is extracted three times with 30 ml of ethyl acetate each time, the combined extracts are dried over sodium sulfate, and the solvent is stripped off in vacuo. The remaining crystalline residue is recrystallized from a little acetonitrile. Yield: 1.5 g of the title compound of m.p. 185° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04363816 |
| 出典データセット | uspto-grants-1982_12 |
| ORD ID | ord-36598b10d8e1476f948130b2687047ed |
| 出典メモ | uspto-grants-1982_12 |