Water → HCID 178466003, 화합물

HRID 392583노트

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HRID 392583 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 22664967HCID 22664967, 화합물HCID 178418918HCID 178418918, 화합물

생성물 1

HCID 178466003HCID 178466003, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

(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).

후처리

  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

출처 및 근거

ORD 기록
ord-99cb3a8d88904992bd31ab98bb1c1a72
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800778B1

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