Water → HCID 178466003、化合物

HRID 392583ノート

反応式

HRID 392583 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[CH:10]=[C:9]([C:14]([C:16]1[N:17]=[CH:18][N:19](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:20]=1)=[O:15])[CH:8]=[CH:7]2)[CH3:2].[CH:40]([Mg]Cl)([CH3:42])[CH3:41].[Cl-].[NH4+].O>C1COCC1>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[CH:10]=[C:9]([C:14]([C:16]1[N:17]=[CH:18][NH:19][CH:20]=1)([OH:15])[CH:40]([CH3:42])[CH3:41])[CH:8]=[CH:7]2)[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 22664967HCID 22664967、化合物HCID 178418918HCID 178418918、化合物

生成物 1

HCID 178466003HCID 178466003、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

(6-Ethoxynaphthalen-2-yl)-(1-trityl-1H-imidazol-4-yl)ketone (3.0 g) was dissolved in THF (45 ml) and a solution (2 M, 4 ml) of isopropyl magnesium chloride in THF was added dropwise under ice-cooling. The mixture was stirred at room temperature for 30 min and saturated aqueous solution (20 ml) of ammonium chloride and water (20 ml) were added. The mixture was extracted with ethyl acetate and the extract was washed with saturated brine, dried and concentrated. The residue was crystallized from ethyl acetate-diisopropyl ether to give the title compound (1.72 g) as a colorless powder. Crystallization mother liquor was purified by silica gel chromatography (eluate, hexane-ethyl acetate=1:2) to give the title compound (0.43 g).

後処理

  1. temperaturecooling
  2. extractionThe mixture was extracted with ethyl acetate
  3. washthe extract was washed with saturated brine
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was crystallized from ethyl acetate-diisopropyl ether

出典と根拠

ORDレコード
ord-99cb3a8d88904992bd31ab98bb1c1a72
出典データセット
uspto-grants-2004_10
特許番号
US06800778B1

反応ノート

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