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苯胺-1-13C → 2-(imidazo[1,2-b]pyridazin-6-ylthio)-N-phenylbenzamide

HRID 1664065
笔记
打印预览

反应方程式

HRID 1664065 反应方程式
[N:1]1[CH:2]=[CH:3][N:4]2[C:9]=1[CH:8]=[CH:7][C:6]([S:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([OH:15])=O)=[N:5]2.[NH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.O.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.C(N(CC)CC)C.[OH-].[Na+]>CN(C)C=O>[N:1]1[CH:2]=[CH:3][N:4]2[C:9]=1[CH:8]=[CH:7][C:6]([S:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:15])=[N:5]2
参与物实验过程后处理来源与证据反应笔记

参与物

8

反应物 6

HCID 6115苯胺-1-13CHCID 8471三乙胺HCID 14798氢氧化钠HCID 27239391-乙基-(3-二甲基氨基丙基)碳酰二亚胺盐酸盐HCID 27960291-羟基苯并三唑合水合物HCID 574410642-(Imidazo[1,2-b]pyridazin-6-ylthio)benzoic acid

产物 1

HCID 57505783
2-(imidazo[1,2-b]pyridazin-6-ylthio)-N-phenylbenzamide
收率 80%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

To a mixture of 2-(imidazo[1,2-b]pyridazin-6-ylthio)benzoic acid (109 mg, 0.40 mmol), aniline (75 mg, 0.81 mmol), 1-hydroxybenzotriazole hydrate (61 mg, 0.40 mmol) and N,N-dimethylformamide (5 mL) were added 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (153 mg, 0.80 mmol) and triethylamine (0.167 mL, 1.20 mmol), and the mixture was stirred at room temperature for 18 hr. A 1N aqueous sodium hydroxide solution was added to the mixture and the mixture was extracted with ethyl acetate. The organic layer was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol=100/0→80/20) and precipitated from ethyl acetate/diisopropyl ether to give the title compound (110 mg, 0.32 mmol, yield 79%) as a white solid.

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. concentrationThe organic layer was concentrated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (ethyl acetate/methanol=100/0→80/20)
  4. customprecipitated from ethyl acetate/diisopropyl ether

来源与证据

ORD记录
ord-640005b434a54b5ab250e96373413975
来源数据集
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08034812B2

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