聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 2-Isopropyl-oxazole-4-carboxylic acid-cyclopropylamide

HRID 5331

反应方程式

HRID 5331 反应方程式
S(Cl)(Cl)=O.[CH:5]([C:8]1[O:9][CH:10]=[C:11]([C:13]([OH:15])=O)[N:12]=1)([CH3:7])[CH3:6].[CH:16]1([NH2:19])[CH2:18][CH2:17]1.O>C1(C)C=CC=CC=1.CN(C)C=O.ClCCl>[CH:16]1([NH:19][C:13]([C:11]2[N:12]=[C:8]([CH:5]([CH3:6])[CH3:7])[O:9][CH:10]=2)=[O:15])[CH2:18][CH2:17]1

参与物

8

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 24386氯化亚砜HCID 69828环丙胺HCID 149648782-异丙基-4,5-二氢恶唑-4-甲酸

产物 1

HCID 156724292-Isopropyl-oxazole-4-carboxylic acid-cyclopropylamide收率 96%

试剂、催化剂与溶剂 3

HCID 1140甲苯溶剂HCID 6228N,N-二甲基甲酰胺溶剂HCID 6344二氯甲烷溶剂2 次

反应条件

温度
80 °C

实验过程

At room temperature, 47.6 g (0.40 mol) of thionyl chloride was dripped into a solution of 31.0 g (0.20 mol) of 2-isopropyloxazole-4-carboxylic acid in 200 ml of toluene and 2 ml of dimethylformamide, and the mixture was stirred for one hour at 80° C. The solvents were stripped off under reduced pressure, the residue was dissolved in 300 ml of dichloromethane, and 24.0 g (0.42 mol) of cyclopropylamine in 20 ml of dichloromethane was dripped in at 0° to 10° C. The mixture was stirred for 12 hours at room temperature, 150 ml of water was added, the phases were separated, the organic phase was washed once with saturated sodium bicarbonate solution and dried over magnesium sulfate, and the solvent was removed under reduced pressure. There was obtained 37.2 g (96%) of 2-isopropyl-oxazole-4-carboxylic acid-cyclopropylamide.

后处理

  1. customAt room temperature
  2. customwas dripped in at 0° to 10° C
  3. stirringThe mixture was stirred for 12 hours at room temperature
  4. customthe phases were separated
  5. washthe organic phase was washed once with saturated sodium bicarbonate solution
  6. dry with materialdried over magnesium sulfate
  7. customthe solvent was removed under reduced pressure

来源与证据

ORD记录
ord-7521a5ff0c9d4c75bde504a8fa790722
来源数据集
uspto-grants-1993_09
专利号
US05244867

关联笔记

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