Pyridine → N-(2,4,6-trimethoxyphenyl)-N'-(4-isopropylcyclohexyl)urea

HRID 37293

反応式

HRID 37293 の反応式
[CH:1]([CH:4]1[CH2:9][CH2:8][CH:7]([N:10]=[C:11]=[O:12])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[CH3:13][O:14][C:15]1[CH:21]=[C:20]([O:22][CH3:23])[CH:19]=[C:18]([O:24][CH3:25])[C:16]=1[NH2:17].N1C=CC=CC=1>C(Cl)(Cl)Cl>[CH3:25][O:24][C:18]1[CH:19]=[C:20]([O:22][CH3:23])[CH:21]=[C:15]([O:14][CH3:13])[C:16]=1[NH:17][C:11]([NH:10][CH:7]1[CH2:8][CH2:9][CH:4]([CH:1]([CH3:3])[CH3:2])[CH2:5][CH2:6]1)=[O:12]

参加物

5

反応物 3

HCID 1049PyridineHCID 842712,4,6-TrimethoxyanilineHCID 199351384-Isopropylcyclohexylisocyanate

生成物 1

HCID 19935028N-(2,4,6-trimethoxyphenyl)-N'-(4-isopropylcyclohexyl)urea

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a solution of 1.6 g of 4-isopropylcyclohexylisocyanate in chloroform is added a solution of 1.8 g of 2,4,6-trimethoxyaniline in chloroform dropwise in the presence of pyridine. The mixture is stirred at room temperature until starting compounds disappear on TLC. The resultant mixture is concentrated and the residue is dissolved in ethyl acetate. The solution is washed with diluted hydrochloric acid, aqueous sodium hydrogencarbonate solution and brine. The organic layer is dried over magnesium sulfate and filtered off. The filtrate is distilled away and the resulting residue is crystallized to give N-(2,4,6-trimethoxyphenyl)-N'-(4-isopropylcyclohexyl)urea.

後処理

  1. concentrationThe resultant mixture is concentrated
  2. dissolutionthe residue is dissolved in ethyl acetate
  3. washThe solution is washed with diluted hydrochloric acid, aqueous sodium hydrogencarbonate solution and brine
  4. dry with materialThe organic layer is dried over magnesium sulfate
  5. filtrationfiltered off
  6. distillationThe filtrate is distilled away
  7. customthe resulting residue is crystallized

出典と根拠

ORDレコード
ord-374741eaee854b63a8671fa751bb72c9
出典データセット
uspto-grants-1995_05
特許番号
US05420164

関連ノート

読み込み中…