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Ammonium Chloride → HCID 178488535, 화합물

HRID 1059141
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HRID 1059141 반응식
[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
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참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 178418918HCID 178418918, 화합물HCID 178488533HCID 178488533, 화합물

생성물 1

HCID 178488535HCID 178488535, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

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온도
-40 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-1fd182301bdd4590b635f20cae3d47ad
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06518257B1

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