Hydrochloric Acid → HCID 178526717, 화합물

HRID 2221417노트

반응식

HRID 2221417 반응식
O1CCCC1.C(CC[N:10]1[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[N:12]=[C:11]1[S:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1)#N.Cl.O>C(OCC)(=O)C>[N+:15]([C:13]1[N:12]=[C:11]([S:18][C:19]2[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=2)[NH:10][CH:14]=1)([O-:17])=[O:16]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8028TetrahydrofuranHCID 230802461-(2-Cyanoethyl)-4-nitro-2-(4-nitrophenylthio)imidazole

생성물 1

HCID 178526717HCID 178526717, 화합물수율 58%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To tetrahydrofuran (1 ml) solution of 1-(2-cyanoethyl)-4-nitro-2-(4-nitrophenylthio)imidazole (27 mg) was added 1,8-diazabicyclo[5.4.0]undecene-7 (0.02 ml) at a room temperature, and stirred at the same temperature for 3 hours. To the reaction mixture were added 1N hydrochloric acid (0.7 ml), water and ethyl acetate, then the organic layer was taken by liquid separation. The ethyl acetate layer was washed with water and an aqueous solution being saturated with sodium chloride, then dried over anhydrous sodium sulfate. The residue obtained by removal of the solvent by distillation was purified by use of a thin layer chromatography (eluent: dichloromethane/ethyl acetate=9/1), there was obtained 4-nitro-2-(4-nitrophenylthio)imidazole (13 mg, yield 58%) as reddish brown powdery product.

후처리

  1. customthe organic layer was taken by liquid separation
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe residue obtained by removal of the solvent by distillation
  5. customwas purified by use of a thin layer chromatography (eluent: dichloromethane/ethyl acetate=9/1)

출처 및 근거

ORD 기록
ord-c58598dd9d1347a2b68a341bc8315278
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368579B2

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