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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → HCID 117864549,化合物

HRID 1486355
笔记
打印预览

反应方程式

HRID 1486355 反应方程式
C(OC(=O)[NH:7][C:8]([CH3:36])([CH2:33][CH2:34][CH3:35])[CH2:9][NH:10][C:11]([C:13]1[C:14]([CH3:32])=[N:15][N:16]2[C:21]([O:22][CH2:23][C:24]3[C:29]([F:30])=[CH:28][CH:27]=[CH:26][N:25]=3)=[CH:20][C:19]([CH3:31])=[CH:18][C:17]=12)=[O:12])(C)(C)C.O.[OH-].[Na+]>FC(F)(F)C(O)=O>[NH2:7][C:8]([CH3:36])([CH2:33][CH2:34][CH3:35])[CH2:9][NH:10][C:11]([C:13]1[C:14]([CH3:32])=[N:15][N:16]2[C:21]([O:22][CH2:23][C:24]3[C:29]([F:30])=[CH:28][CH:27]=[CH:26][N:25]=3)=[CH:20][C:19]([CH3:31])=[CH:18][C:17]=12)=[O:12]
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 14798氢氧化钠HCID 117864682rac-{1-[({7-[(3-Fluoropyridin-2-yl)methoxy]-2,5-dimethylpyrazolo[1,5-a]pyridin-3-yl}carbonyl)amino]-2-methylpentan-2-yl}carbamic Acid tert-butyl Ester

产物 1

HCID 117864549HCID 117864549,化合物收率 10%

试剂、催化剂与溶剂 1

HCID 6422三氟乙酸溶剂

反应条件

温度
50 °C

实验过程

20 mg (0.039 mmol) of rac-{1-[({7-[(3-fluoropyridin-2-yl)methoxy]-2,5-dimethylpyrazolo[1,5-a]pyridin-3-yl}carbonyl)amino]-2-methylpentan-2-yl}carbamic acid tert-butyl ester (Example 144A) were dissolved in 1 ml of trifluoroacetic acid. The reaction mixture was heated to 50° C. for 1 hour. Water was added, and the pH was adjusted to −9 with 2 N sodium hydroxide solution. The aqueous phase was extracted with dichloromethane, separated off and concentrated under reduced pressure. The residue was purified by preparative HPLC chromatography (Method 21), which gave 1.59 mg (10% yield) of the target compound.

后处理

  1. extractionThe aqueous phase was extracted with dichloromethane
  2. customseparated off
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by preparative HPLC chromatography (Method 21), which

来源与证据

ORD记录
ord-7256099ea0c543a9a62d014201b7d3f1
来源数据集
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
专利号
US09422285B2

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记