聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → HCID 20364661，化合物

HRID 225777

反应方程式

HRID 225777 反应方程式
[C:1]1([SH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:9]1[S:10][C:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:12]([CH3:14])[N:13]=1.O>CN(C)C=O>[CH3:14][C:12]1[N:13]=[C:9]([S:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[S:10][C:11]=1[C:15]([O:17][CH2:18][CH3:19])=[O:16]

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 7969苯硫酚HCID 594903Ethyl 2-chloro-4-methyl-1,3-thiazole-5-carboxylate

产物 1

HCID 20364661HCID 20364661，化合物

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂2 次

实验过程

Thiophenol (1.90 ml) was dissolved in N,N-dimethylformamide (10 ml) Sodium hydride (60% oil suspension, 740 mg) was added by portions under ice-cooling, and the mixture was stirred at room temperature for 15 min. Thereafter, a solution of ethyl 2-chloro-4-methylthiazole-5-carboxylate (3.05 g) in N,N-dimethylformamide (10 ml) was added dropwise, and the mixture was stirred at the same temperature for 20 min. Water (50 ml) was added to the reaction mixture, and the mixture was extracted with ethyl acetate (50 ml). The ethyl acetate layer was washed twice with water (50 ml) and then with saturated brine (30 ml), and dried (Na2SO4). Ethyl acetate was evaporated under reduced pressure and the obtained residue was purified by column chromatography to give ethyl 4-methyl-2-phenylsulfanylthiazole-5-carboxylate (3.85 g).

后处理

  1. additionwas added by portions under ice-
  2. temperaturecooling
  3. stirringthe mixture was stirred at the same temperature for 20 min
  4. extractionthe mixture was extracted with ethyl acetate (50 ml)
  5. washThe ethyl acetate layer was washed twice with water (50 ml)
  6. dry with materialwith saturated brine (30 ml), and dried (Na2SO4)
  7. customEthyl acetate was evaporated under reduced pressure
  8. customthe obtained residue was purified by column chromatography

来源与证据

ORD记录
ord-d4501c3e611d4c658621a081bd183b26
来源数据集
uspto-grants-2009_07
专利号
US07557123B2

关联笔记

加载中…