3-羟基吡咯烷 → 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

HRID 53543

反应方程式

HRID 53543 反应方程式
Cl[C:2]1[CH:3]=[C:4]([CH3:20])[C:5]2[NH:6][C:7](=[O:19])[C:8]3[CH:18]=[CH:17][CH:16]=[N:15][C:9]=3[N:10]([CH2:13][CH3:14])[C:11]=2[N:12]=1.[OH:21][CH:22]1[CH2:26][CH2:25][NH:24][CH2:23]1>O>[CH2:13]([N:10]1[C:9]2[N:15]=[CH:16][CH:17]=[CH:18][C:8]=2[C:7](=[O:19])[NH:6][C:5]2[C:4]([CH3:20])=[CH:3][C:2]([N:24]3[CH2:25][CH2:26][CH:22]([OH:21])[CH2:23]3)=[N:12][C:11]1=2)[CH3:14]

参与物

4

反应物 2

HCID 982103-羟基吡咯烷HCID 463144Dipyridodiazepinone deriv. 15

产物 1

HCID 46354911-Ethyl-2-(3-hydroxypyrrolidin-1-yl)-4-methyl-5,11-dihydro-6H-dipyrido[2,3-e:3',2'-b][1,4]diazepin-6-one

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
170 °C

实验过程

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.

后处理

  1. temperatureAfter cooling to room temperature the mixture
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed
  4. customdried
  5. customevaporated

来源与证据

ORD记录
ord-85aae3c011414557809e137dd866b50d
来源数据集
uspto-grants-1997_04
专利号
US05620974

关联笔记

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