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氢氧化钠 → 2-(4-Fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinic acid

HRID 1908274
笔记
打印预览

反应方程式

HRID 1908274 反应方程式
[F:1][C:2]1[C:3]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[N:4][N:5]([C:7]2[N:17]=[CH:16][CH:15]=[CH:14][C:8]=2[C:9]([O:11]CC)=[O:10])[CH:6]=1.[OH-].[Na+]>CO>[F:1][C:2]1[C:3]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[N:4][N:5]([C:7]2[N:17]=[CH:16][CH:15]=[CH:14][C:8]=2[C:9]([OH:11])=[O:10])[CH:6]=1
参与物实验过程后处理来源与证据反应笔记

参与物

4

反应物 2

HCID 14798氢氧化钠HCID 67238757ethyl 2-(4-fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinate

产物 1

HCID 672390012-(4-Fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinic acid收率 90.7%

试剂、催化剂与溶剂 1

HCID 887Methanol溶剂

实验过程

To ethyl 2-(4-fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinate (1.49 g, 4.79 mmol) in methanol (40 ml) 8.5 ml of an aqueous 2 m NaOH-solution (17 mmol) was added dropwise at 10° C., and the mixture was stirred for 2 h at room temperature and then for 3 h at 65° C. After completion of the reaction the mixture was concentrated under reduced pressure, dissolved in water and acidified using 2 n HCl. The precipitate formed was filtered off, washed with water and dried to give 1.23 g of a white amorphous solid; ESI-MS [M+H]+: 284.1.

后处理

  1. waitfor 3 h at 65° C
  2. customAfter completion of the reaction the mixture
  3. concentrationwas concentrated under reduced pressure
  4. dissolutiondissolved in water
  5. customThe precipitate formed
  6. filtrationwas filtered off
  7. washwashed with water
  8. customdried

来源与证据

ORD记录
ord-2c44cc29812d48248647ce317ed06064
来源数据集
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08598211B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记