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盐酸 → 6-Amino-5-{3-[(2,5-dimethyl-2H-pyrazole-3-carbonyl)-amino]-phenylethynyl}-nicotinic acid

HRID 607485
笔记
打印预览

反应方程式

HRID 607485 反应方程式
[NH2:1][C:2]1[C:11]([C:12]#[C:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([NH:20][C:21]([C:23]3[N:27]([CH3:28])[N:26]=[C:25]([CH3:29])[CH:24]=3)=[O:22])[CH:15]=2)=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][N:3]=1.[OH-].[K+].Cl>CO.O.[Cl-].[Na+].O>[NH2:1][C:2]1[C:11]([C:12]#[C:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([NH:20][C:21]([C:23]3[N:27]([CH3:28])[N:26]=[C:25]([CH3:29])[CH:24]=3)=[O:22])[CH:15]=2)=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1
参与物实验过程后处理来源与证据反应笔记

参与物

6

反应物 3

HCID 313盐酸HCID 14797氢氧化钾HCID 57657963methyl 6-amino-5-[(3-{[(1,3-dimethyl-1H-pyrazol-5-yl)carbonyl]amino}phenyl)ethynyl]nicotinate

产物 1

HCID 576578676-Amino-5-{3-[(2,5-dimethyl-2H-pyrazole-3-carbonyl)-amino]-phenylethynyl}-nicotinic acid收率 84%

试剂、催化剂与溶剂 2

HCID 22242641Methanol--water (1/1)溶剂
HCID 57417360
Sodium chloride; water
溶剂

实验过程

A solution of methyl 6-amino-5-[(3-{[(1,3-dimethyl-1H-pyrazol-5-yl)carbonyl]amino}phenyl)ethynyl]nicotinate (51 mg, 0.13 mmol) and KOH (37 mg, 0.65 mmol) in 4.0 ml MeOH:H2O (3:1) was heated at 65□C. for 1 hour 40 minutes. The pH of the mixture was adjusted to pH 4 using 10% HCl, brine added, and the aqueous extracted with EtOAc. The combined EtOAc layers were dried with anhydrous Na2SO4 and rotary evaporated. The light yellow solid was triturated with hot EtOAc to give the title compound as an off-white solid (41 mg, 84%).

后处理

  1. additionadded
  2. extractionthe aqueous extracted with EtOAc
  3. dry with materialThe combined EtOAc layers were dried with anhydrous Na2SO4 and rotary evaporated
  4. customThe light yellow solid was triturated with hot EtOAc

来源与证据

ORD记录
ord-b15b63f6213d495a8f3710f273887243
来源数据集
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
专利号
US07915443B2

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