参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 3-羟基吡咯烷 | HCID 98210 | — |
| 反应物 | Dipyridodiazepinone deriv. 15 | HCID 463144 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | 11-Ethyl-2-(3-hydroxypyrrolidin-1-yl)-4-methyl-5,11-dihydro-6H-dipyrido[2,3-e:3',2'-b][1,4]diazepin-6-one | HCID 463549 | — |
反应步骤
A suspension of the 2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.14 g) in 3-hydroxypyrrolidine (0.29 g) in an open test tube was heated at 170° C. for 30 minutes. After cooling to room temperature the mixture was diluted with water and extracted with ethyl acetate. The organic phase was washed, dried, and evaporated. Chromatography over silica gel with ethyl acetate gave the title compound, which crystallized from ethyl acetate. Yield, 0.12 g, m.p. 131°-134° C.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US05620974 |
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| 来源数据集 | uspto-grants-1997_04 |
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| ORD ID | ord-85aae3c011414557809e137dd866b50d |
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| 来源说明 | uspto-grants-1997_04 |
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