Water → HCID 178442815, 화합물

HRID 274867

반응식

HRID 274867 반응식
[CH2:1]([C:13]1[CH:19]=[CH:18][C:16]([NH2:17])=[CH:15][CH:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C([O:22][C:23]([CH:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1)=O)C.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1C=CC=CC=1>[CH2:1]([C:13]1[CH:14]=[C:15]2[C:16]([N:17]=[C:26]3[C:25](=[C:23]2[OH:22])[CH2:30][CH2:29][CH2:28][CH2:27]3)=[CH:18][CH:19]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

참가 물질

6

반응물 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 77014-DodecylanilineHCID 18686Ethyl cyclohexanoate

생성물 1

HCID 178442815HCID 178442815, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

4-Dodecylaniline (15.7 g) was dissolved in 100 mL of benzene and then 2-ethoxycarbonylcyclohexane (10.2 g) was added, followed by 0.20 g of p-toluenesulfonic acid. The reaction mixture was stirred for three days and then refluxed for 2 hours with the separation of H2O. The benzene was evaporated from this mixture, which was then dissolved in 100 mL of phenyl ether and refluxed for 45 minutes. At the end of this time the reaction mixture was allowed to cool and the precipitated product was filtered off. This crude product was purified by flash chromatography (20% ethyl acetate/CH2Cl2) and then recrystallized from 1,2-dichloroethane/methanol to give 1.31 g, mp 225°-226°.

후처리

  1. customThe benzene was evaporated from this mixture, which
  2. dissolutionwas then dissolved in 100 mL of phenyl ether
  3. temperaturerefluxed for 45 minutes
  4. temperatureto cool
  5. filtrationthe precipitated product was filtered off
  6. customThis crude product was purified by flash chromatography (20% ethyl acetate/CH2Cl2)
  7. customrecrystallized from 1,2-dichloroethane/methanol
  8. customto give 1.31 g, mp 225°-226°

출처 및 근거

ORD 기록
ord-4f0bcb9ef9e144f8b3e9ffbc7a97c647
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05391553

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