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Potassium Carbonate → 4-(3-Bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Propanoyl chloride, 3-bromo- | HCID 84944 | — |
| 反応物 | 1,3-Dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one | HCID 18975980 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(3-Bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one | HCID 20515487 | 70.6% |
反応手順
A solution of 3.42 g of 3-bromopropionyl chloride in 20 ml of dioxane is added dropwise to 4.54 g of 1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one, 5.0 g of powdered anhydrous potassium carbonate and 80 ml of dry dioxane in the course of 10 minutes at from 50° to 60° C., and the mixture is stirred at this temperature for a further 2 hours. The solvent is stripped off in vacuo, and the resulting solid residue is stirred with 300 ml of ice water and filtered off. 5.1 g of the title compound of m.p. 194° to 195° C. (D.) are obtained after recrystallization from isopropanol.
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-b6b3a5d6631842f8bfcdd9faff645788 |
| 出典メモ | uspto-grants-1982_12 |