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

HRID 37293노트

반응식

HRID 37293 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-374741eaee854b63a8671fa751bb72c9
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420164

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