聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → N-(2-Aminoethyl)-N'(3,5-dimethoxyphenyl)thiourea

HRID 1193523

反应方程式

HRID 1193523 反应方程式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:11]=[C:12]=[S:13])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.[CH2:14]([NH2:17])[CH2:15][NH2:16].O>CCOCC>[NH2:16][CH2:15][CH2:14][NH:17][C:12]([NH:11][C:5]1[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1)=[S:13]

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 3301乙二胺HCID 1454223,5-二甲氧基苯基异硫氰酸酯

产物 1

HCID 13604911N-(2-Aminoethyl)-N'(3,5-dimethoxyphenyl)thiourea

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂

反应条件

温度
50 °C

实验过程

A slurry of 9.75 g (0.05 mole) of 3,5-dimethoxyphenyl isothiocyanate in 27 ml of ether was added dropwise to a stirred solution of 3.0 g (0.05 mole) of ethylenediamine at room temperature. A five-degree rise in temperature was noted at the start of the one hour addition period. A solid appeared during the addition, and stirring was continued for 2.5 hours. The batch was allowed to stand overnight, and 100 ml of H2O was added. The solid was removed by filtration and the filtrate acidified with 4.5 ml of concentrated HCl and evaporated to dryness on the steam bath. The residue was sonicated with 100 ml of water and warmed to 50° C. for 10 minutes. This was filtered and basified to pH 10 with 10% NaOH. This gave 2.6 g of 14, m.p. 125°-126° C. Analysis satisfactory for C11H17N3O2S.

后处理

  1. additionA five-degree rise in temperature was noted at the start of the one hour addition period
  2. additionA solid appeared during the addition
  3. waitto stand overnight
  4. customThe solid was removed by filtration
  5. customevaporated to dryness on the steam bath
  6. customThe residue was sonicated with 100 ml of water
  7. filtrationThis was filtered

来源与证据

ORD记录
ord-55c9c6c8b341407bb24a3bb2999b6d79
来源数据集
uspto-grants-1989_03
专利号
US04810725

关联笔记

加载中…