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Ammonium Chloride → HCID 178488535、化合物

HRID 1059141
ノート
印刷プレビュー

反応式

HRID 1059141 の反応式
[NH:1]1[CH:5]=[C:4]([C:6]([C:8]2[CH:9]=[C:10]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:11]=[CH:12][C:13]=2[O:14][CH3:15])=[O:7])[N:3]=[CH:2]1.[CH:22]([Mg]Cl)([CH3:24])[CH3:23].[Cl-].[NH4+]>C1COCC1.O>[NH:1]1[CH:5]=[C:4]([C:6]([C:8]2[CH:9]=[C:10]([C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH:11]=[CH:12][C:13]=2[O:14][CH3:15])([OH:7])[CH:22]([CH3:24])[CH3:23])[N:3]=[CH:2]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 3

HCID 25517Ammonium ChlorideHCID 178418918HCID 178418918、化合物HCID 178488533HCID 178488533、化合物

生成物 1

HCID 178488535HCID 178488535、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-40 °C

実験手順

1H-Imidazol-4-yl(4-methoxy[1,1′-biphenyl]-3-yl)methanone (0.62 g) was dissolved in THF (15 ml) and the mixture was cooled to −40° C. A solution (0.6 M; 15 ml) of isopropyl magnesium chloride in THF was slowly added dropwise and the mixture was warmed to room temperature. The mixture was stirred for 1 h and thereto was added saturated aqueous ammonium chloride solution. The mixture was diluted with water and extracted with ethyl acetate. The extract was dried and concentrated. The obtained residue was purified by silica gel column chomatography (eluent, dichloromethane:methanol=40:1) to give the colorless amorphous title compound (0.16 g).

後処理

  1. temperaturethe mixture was warmed to room temperature
  2. extractionextracted with ethyl acetate
  3. customThe extract was dried
  4. concentrationconcentrated
  5. customThe obtained residue was purified by silica gel column chomatography (eluent, dichloromethane:methanol=40:1)

出典と根拠

ORDレコード
ord-1fd182301bdd4590b635f20cae3d47ad
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06518257B1

反応ノート

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