海萝胶 → HCID 178418398，化合物

HRID 1028

反应方程式

HRID 1028 反应方程式
Cl[C:2]1[C:7]([Br:8])=[C:6]([NH:9][C@H:10]2[CH2:15][CH2:14][C@@H:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:12][CH2:11]2)[CH:5]=[CH:4][N:3]=1.[CH3:22][O-:23].[Na+].O.Cl>CN(C)C=O.CO>[CH3:22][O:23][C:2]1[C:7]([Br:8])=[C:6]([NH:9][C@H:10]2[CH2:15][CH2:14][C@@H:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:12][CH2:11]2)[CH:5]=[CH:4][N:3]=1

参与物

7

反应物 4

HCID 313海萝胶HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 10942334甲醇钠HCID 178418294HCID 178418294，化合物

产物 1

HCID 178418398HCID 178418398，化合物

试剂、催化剂与溶剂 2

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂HCID 6228N,N-二甲基甲酰胺溶剂

反应条件

温度
80 °C

实验过程

2.21 g (6.04 mmol) of 2-chloro-3-bromo-4-(cis-4-phenylcyclohexylamino)pyridine in 30 ml of dimethylformamide are treated with 4.31 ml of 30% strength solution of sodium methoxide in methanol and the mixture is heated at 80° C. for 1 hour. After cooling, water is added, the mixture is adjusted to pH 8 using 1/2 conc. hydrochloric acid and the reaction product is extracted with ethyl acetate. For purification it is chromatographed. Yield: 1.72 g (79%); Rf =0.4 (diisopropyl ether)

后处理

  1. temperatureAfter cooling
  2. extractionthe reaction product is extracted with ethyl acetate
  3. customFor purification it
  4. customis chromatographed

来源与证据

ORD记录
ord-5a04f014ea6d40c2b125f6974f5951e3
来源数据集
uspto-grants-1998_03
专利号
US05723450

关联笔记

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