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Ethyl chloroformate → HCID 14877394, 화합물

HRID 1608213
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HRID 1608213 반응식
C([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH2:14][N:15]2[C:19](=[O:20])[C:18]3=[CH:21][CH:22]=[CH:23][CH:24]=[C:17]3[C:16]2=[O:25])[CH2:9]1)C1C=CC=CC=1.Cl[C:27]([O:29][CH2:30][CH3:31])=[O:28]>C1(C)C=CC=CC=1>[CH2:30]([O:29][C:27]([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH2:14][N:15]2[C:16](=[O:25])[C:17]3=[CH:24][CH:23]=[CH:22][CH:21]=[C:18]3[C:19]2=[O:20])[CH2:9]1)=[O:28])[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 117245602-((4-benzylmorpholin-2-yl)methyl)-2,3-dihydro-1H-isoindole-1,3-dione

생성물 1

HCID 14877394HCID 14877394, 화합물수율 97.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a stirred solution of N-[(4-benzyl-2-morpholinyl)methyl]phthalimide (30.0 g) in toluene (200 ml), ethyl chloroformate (19.4 g) is added dropwise at 60° C., and the mixture is refluxed with stirring for 1 hour. The reaction mixture is washed successively with water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The solvent is distilled off under reduced pressure, and the residue is recrystallized from isopropyl alcohol-diethyl ether to give N-[(4-ethoxycarbonyl-2-morpholinyl)methyl]phthalimide (27.8 g), mp 113°-115° C.

후처리

  1. temperaturethe mixture is refluxed
  2. washThe reaction mixture is washed successively with water and saturated aqueous sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent is distilled off under reduced pressure
  5. customthe residue is recrystallized from isopropyl alcohol-diethyl ether

출처 및 근거

ORD 기록
ord-e7ca7fc8f7e744cf8ef43d67c19680e6
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870074

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