氢溴酸 → HCID 83698021，化合物

HRID 2411227

反应方程式

HRID 2411227 反应方程式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[CH:4][C:3]=1[N:9]1[CH2:14][CH2:13][N:12](S(C2C=CC(C)=CC=2)(=O)=O)[CH2:11][CH2:10]1.Br.[OH-].[Na+]>C(O)(=O)C>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[CH:4][C:3]=1[N:9]1[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]1

参与物

5

反应物 3

HCID 260氢溴酸HCID 14798二甲基对苯二胺二盐酸HCID 712521811-(4,6-Dimethylpyridin-3-yl)-4-(toluene-4-sulfonyl)piperazine

产物 1

HCID 83698021HCID 83698021，化合物收率 62.3%

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂

反应条件

温度
100 °C

实验过程

To 5-amino-2,4-dimethylpyridine (883 mg) were added N,N-diisopropylethylamine (2.1 mL) and N,N-bis(2-chloroethyl)-p-toluenesulfonamide (2.08 g), and the mixture was stirred with heating under reflux. After completion of the reaction, water was added to the reaction mixture, the mixture was extracted with chloroform, and the solvent was evaporated. The obtained residue was purified by column chromatography (chloroform:methanol) to give 1-(4,6-dimethylpyridin-3-yl)-4-(toluene-4-sulfonyl)piperazine (380 mg). The obtained 1-(4,6-dimethylpyridin-3-yl)-4-(toluene-4-sulfonyl)piperazine (380 mg) was dissolved in acetic acid (2 mL), 40% hydrobromic acid (2 mL) was added, and the mixture was stirred at 100° C. After completion of the reaction, the reaction mixture was neutralized with aqueous sodium hydroxide solution, and the mixture was extracted with ethyl acetate. The solvent was evaporated from the organic layer to give the title compound (131 mg).

后处理

  1. customAfter completion of the reaction
  2. extractionthe mixture was extracted with ethyl acetate
  3. customThe solvent was evaporated from the organic layer

来源与证据

ORD记录
ord-567da05e6a364c3f873dd3bbccd9f107
来源数据集
uspto-grants-2014_08
专利号
US08816079B2

关联笔记

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