Water → HCID 68674456、化合物

HRID 1927685ノート

反応式

HRID 1927685 の反応式
[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

参加物

7

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 83372Dimethylsulphamoyl chlorideHCID 178506558HCID 178506558、化合物

生成物 1

HCID 68674456HCID 68674456、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 21584124Propan-2-one--dichloromethane (1/1)溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-adbb8d9ba11c4b7485a0d4d78bb10712
出典データセット
uspto-grants-2012_05
特許番号
US08183275B2

反応ノート

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