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Ammonia → HCID 178424632、化合物

HRID 619680
ノート
印刷プレビュー

反応式

HRID 619680 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 102542,4,6-TrimethylbenzaldehydeHCID 517165Ammonium AcetateHCID 21847014HCID 21847014、化合物

生成物 1

HCID 178424632HCID 178424632、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-580ac4d43c5f4a5da0ccbe37690834c4
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05959113

反応ノート

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