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4-Iodobenzonitrile → 4-[2-(1-trityl-1H-imidazol-4-ylmethoxy)acetyl]benzonitrile

HRID 1360136
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HRID 1360136 반응식
I[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[CH:10]([Mg]Cl)([CH3:12])[CH3:11].CON(C)[C:18](=[O:46])[CH2:19][O:20][CH2:21][C:22]1[N:23]=[CH:24][N:25]([C:27](C2C=CC=CC=2)([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)C2C=CC=CC=2)[CH:26]=1>O1CCCC1>[C:27]([N:25]1[CH:26]=[C:22]([CH2:21][O:20][CH2:19][C:18]([C:2]2[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=2)=[O:46])[N:23]=[CH:24]1)([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)([C:10]1[CH:12]=[CH:26][CH:22]=[CH:21][CH:11]=1)[C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 764674-IodobenzonitrileHCID 86632953N-methoxy-N-methyl-2-(1-trityl-1H-imidazol-4-ylmethoxy)acetamideHCID 178418918HCID 178418918, 화합물

생성물 1

HCID 667823264-[2-(1-trityl-1H-imidazol-4-ylmethoxy)acetyl]benzonitrile

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
-30 °C

실험 절차

A solution of 14 mmol of 4-iodobenzonitrile [3058-39-7] in 20 ml of tetrahydrofuran is cooled to −30° C., and 14.80 mmol of i-propylmagnesium chloride (2M in tetrahydrofuran) are added. The mixture is stirred at −30° C. for 60 minutes and a solution, precooled to −30° C., of 10.0 mmol of N-methoxy-N-methyl-2-(1-trityl-1H-imidazol-4-ylmethoxy)acetamide in 30 ml of tetrahydrofuran is added. The mixture is stirred at −30° C. for 30 minutes, and then the reaction mixture is warmed to room temperature and quenched with saturated aqueous ammonium chloride, solution. The phases are separated, and the aqueous phase is extracted with ethyl acetate (3×). The combined organic phases are washed with brine, dried with magnesium sulphate and evaporated. The title compound is identified from the residue on the basis of the Rf by flash chromatography (SiO2 60F).

후처리

  1. additionis added
  2. stirringThe mixture is stirred at −30° C. for 30 minutes
  3. temperaturethe reaction mixture is warmed to room temperature
  4. customquenched with saturated aqueous ammonium chloride, solution
  5. customThe phases are separated
  6. extractionthe aqueous phase is extracted with ethyl acetate (3×)
  7. washThe combined organic phases are washed with brine
  8. dry with materialdried with magnesium sulphate
  9. customevaporated

출처 및 근거

ORD 기록
ord-c3e962acbe3745babacef3a6a7070b29
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07879847B2

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