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Hydrochloric Acid → HCID 20827741, 화합물

HRID 495637
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HRID 495637 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9](=[O:13])[O:10][CH2:11][CH3:12])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].Cl[C:17]1[C:22]([N+:23]([O-:25])=[O:24])=[CH:21][C:20]([N+:26]([O-:28])=[O:27])=[CH:19][C:18]=1[C:29]([F:32])([F:31])[F:30].Cl>COCCOCCOC>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]([C:17]2[C:18]([C:29]([F:31])([F:32])[F:30])=[CH:19][C:20]([N+:26]([O-:28])=[O:27])=[CH:21][C:22]=2[N+:23]([O-:25])=[O:24])[C:9](=[O:13])[O:10][CH2:11][CH3:12])[CH:5]=[CH:6][CH:7]=1
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참가 물질

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반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 67851Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)-HCID 247900Ethyl (3-chlorophenyl)carbamate

생성물 1

HCID 20827741HCID 20827741, 화합물수율 42.3%

시약·촉매·용매 1

HCID 8150
Diglyme
용매

실험 절차

Ethyl 3-chlorophenylcarbamate (1.0256 g) was dissolved in diglyme (3 ml), and to the solution were added sodium hydride (205.5 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (1.1583 g). The reaction mixture was stirred at room temperature for 4 hours. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution, and then saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=5:1) and recrystallized from hexane-ethyl acetate to give the title compound (0.7854 g, 42%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution
  3. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=5:1)
  6. customrecrystallized from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-e74410f091254aba84fd9b554c3b23cd
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06939887B2

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