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Ammonia → HCID 178424632, 화합물

HRID 619680
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HRID 619680 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[C:9]([C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)=O)=[CH:4][CH:3]=1.[CH3:18][C:19]1[CH:26]=[C:25]([CH3:27])[CH:24]=[C:23]([CH3:28])[C:20]=1[CH:21]=O.C([O-])(=O)C.[NH4+:33].[NH3:34]>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:34][C:21]([C:20]3[C:19]([CH3:18])=[CH:26][C:25]([CH3:27])=[CH:24][C:23]=3[CH3:28])=[N:33][C:9]=2[C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 102542,4,6-TrimethylbenzaldehydeHCID 517165Ammonium AcetateHCID 21847014HCID 21847014, 화합물

생성물 1

HCID 178424632HCID 178424632, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

A mixture of 12.3 g of 1-(4-chlorophenyl)-2-pyridin-4-yl-ethanedione and 7.4 g of 2,4,6-trimethylbenzaldehyde in 125 ml of acetic acid containing 40 g of ammonium acetate was stirred at 100° C. for 2 hours, then left to cool to room temperature. The mixture was poured into a mixture of 300 ml of ice-water and 200 ml of concentrated ammonia solution and the mixture was extracted three times with ethyl acetate. After drying over anhydrous magnesium sulphate the solvent was evaporated. The residue was purified by chromatography on silica gel with dichloromethane/methanol (9:1) and crystallized from ethyl acetate to yield 6.7 g of 4-[5-(4-chlorophenyl)-2-(2,4,6-trimethyphenyl)imidazol-4-yl]pyridine, m.p. 275° C.

후처리

  1. waitleft
  2. temperatureto cool to room temperature
  3. extractionthe mixture was extracted three times with ethyl acetate
  4. dry with materialAfter drying over anhydrous magnesium sulphate the solvent
  5. customwas evaporated
  6. customThe residue was purified by chromatography on silica gel with dichloromethane/methanol (9:1)
  7. customcrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-580ac4d43c5f4a5da0ccbe37690834c4
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05959113

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