Water → HCID 68674456, 화합물

HRID 1927685노트

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HRID 1927685 반응식
[H-].[Na+].[I:3][C:4]1[N:5]=[C:6]([CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)=[CH:13][CH:12]=2)[NH:7][CH:8]=1.[CH3:23][N:24]([CH3:29])[S:25](Cl)(=[O:27])=[O:26].O>CN(C)C=O.C(Cl)Cl.CC(C)=O>[I:3][C:4]1[N:5]=[C:6]([CH2:9][CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)=[CH:15][CH:16]=2)[N:7]([S:25]([N:24]([CH3:29])[CH3:23])(=[O:27])=[O:26])[CH:8]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 83372Dimethylsulphamoyl chlorideHCID 178506558HCID 178506558, 화합물

생성물 1

HCID 68674456HCID 68674456, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 21584124Propan-2-one--dichloromethane (1/1)용매

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온도
0 °C

실험 절차

Sodium hydride (384 mg, 16 mmol) was added to a solution of 2-{4-[2-(4-iodo-1H-imidazol-2-yl)ethyl]phenyl}pyridine (5 g, 13.3 mmol) in dimethylformamide (100 mL) at 0° C. After stirring at 0° C. for 1 hr, dimethylsulfamoyl chloride (2.15 mL, 20 mmol) was added. After stirring at rt overnight, the reaction mixture was poured into water and extracted with ethyl acetate. The extracts were washed with brine, dried (sodium sulfate) and concentrated to give a residue. Chromatography of the residue over silica gel eluting with 0-20% acetone methylene chloride afforded 4-iodo-N,N-dimethyl-2-[2-(4-pyridin-2-ylphenyl)ethyl]-1H-imidazole-1-sulfonamide.

후처리

  1. stirringAfter stirring at rt overnight
  2. extractionextracted with ethyl acetate
  3. washThe extracts were washed with brine
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated
  6. customto give a residue

출처 및 근거

ORD 기록
ord-adbb8d9ba11c4b7485a0d4d78bb10712
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183275B2

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