Triethylamine → N-2-ethyl-cyclohexylamino-3,4,5-trimethoxy-benzoate hyrochloride

HRID 596233노트

반응식

HRID 596233 반응식
[CH:1]1([NH:7][CH:8](O)[CH3:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH:26]=[C:27]([O:31][CH3:32])[C:28]=1[O:29][CH3:30])[C:23]([Cl:25])=[O:24].C(OCC)(=[O:35])C>>[CH3:9][CH2:8][N:7]([C:21]1[C:20]([O:19][CH3:18])=[C:28]([O:29][CH3:30])[C:27]([O:31][CH3:32])=[CH:26][C:22]=1[C:23]([O-:35])=[O:24])[CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[ClH:25]

참가 물질

5

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl Acetate2회HCID 78282Benzoyl chloride, 3,4,5-trimethoxy-HCID 20285879Cyclohexylamino ethanol

생성물 1

HCID 86734520N-2-ethyl-cyclohexylamino-3,4,5-trimethoxy-benzoate hyrochloride

실험 절차

2.86 g. of cyclohexylamino ethanol and 2.02 g. of triethyl amine are dissolved in 30 ml. of anhydrous ethyl acetate. A solution of 4.6 g. of 3,4,5-trimethoxybenzoyl-chloride and 20 ml. of anhydrous ethyl acetate are added under stirring and boiling. The reaction mixture is refluxed for 2 hours, whereafter it is cooled and the precipitate is filtered off by suction and washed with ethyl acetate. The ethyl acetate solution is saturated with gaseous hydrochloric acid. The mixture is refluxed for an hour. On cooling white crystals precipitate. Thus N-2-ethyl-cyclohexylamino-3,4,5-trimethoxy-benzoate-hyrochloride is obtained. M.p.: 209° - 210° C.

후처리

  1. temperatureThe reaction mixture is refluxed for 2 hours, whereafter it
  2. temperatureis cooled
  3. filtrationthe precipitate is filtered off by suction
  4. washwashed with ethyl acetate
  5. temperatureThe mixture is refluxed for an hour
  6. temperatureOn cooling white crystals precipitate

출처 및 근거

ORD 기록
ord-eb1b2547ed2e407689cd187d69bedb1f
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04010193

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