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Ethyl chloroformate → HCID 21243401, 화합물

HRID 621614
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HRID 621614 반응식
[CH3:1][N:2]([CH2:4][CH:5]([CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=1)C.Cl[C:26]([O:28][CH2:29][CH3:30])=[O:27]>C1(C)C=CC=CC=1>[C:26]([N:2]([CH2:4][CH:5]([CH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:15])([F:16])[F:17])=[CH:10][CH:9]=1)[CH3:1])([O:28][CH2:29][CH3:30])=[O:27]
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참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 13653935N,N-dimethyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine

생성물 1

HCID 21243401HCID 21243401, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of N,N-dimethyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine (22.0 g) and ethyl chloroformate (34.1 g, 30.0 ml) in dry toluene (200 ml) is refluxed for 72 hours. The reaction mixture is cooled to room temperature, and the solvent removed under reduced pressure. Water (200 ml) is added, and the mixture extracted with dichloromethane (2×150 ml). The combined dichloromethane extracts are washed with 2N hydrochloric acid (200 ml) and water (200 ml), and dried over magnesium sulfate. The solvent is removed under reduced pressure to give N-carbethoxy-N-methyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine as an oil, which is used without purification for the next synthetic step above.

후처리

  1. customthe solvent removed under reduced pressure
  2. additionWater (200 ml) is added
  3. extractionthe mixture extracted with dichloromethane (2×150 ml)
  4. washThe combined dichloromethane extracts are washed with 2N hydrochloric acid (200 ml) and water (200 ml)
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-ba8245c1ff80494b9eea00a9ef24cb99
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04824868

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