Sodium Iodide → HCID 178466792、化合物

HRID 726255

反応式

HRID 726255 の反応式
[CH3:1][C:2]([C:4]1[CH:5]=[CH:6][C:7]([OH:10])=[CH:8][CH:9]=1)=[O:3].Cl.Cl[CH2:13][CH2:14][C:15]1[N:16]=[CH:17][NH:18][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O>[C:2]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:13][CH2:14][C:15]2[N:16]=[CH:17][NH:18][CH:19]=2)=[CH:6][CH:5]=1)(=[O:3])[CH3:1]

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 74694'-HydroxyacetophenoneHCID 11430Potassium CarbonateHCID 1784785704-(2-chloroethyl)-1H-imidazole hydrochloride

生成物 1

HCID 178466792HCID 178466792、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

816 mg (6 mmol) of 4-hydroxyacetophenone, 251 mg (1.5 mmol) of 4-[2-chloroethyl]-1H-imidazole hydrochloride, 500 mg (3.6 mmol) of potassium carbonate and sodium iodide (catalyst) are stirred at 80° C. for 5 days in 5 ml of dimethylformamide. The reaction mixture is cooled, filtered and the filtrate is evaporated under reduced pressure to give an oily residue, from which 4-hydroxyacetophenone is extracted with ether at pH=1. Subsequent extraction with ethyl acetate at pH=9 gives the title compound. The latter was treated with oxalic acid in 2-propanol to give the oxalate of the title compound which is crystallized from a methanol/ether (10/1) mixture, M.p.: 178°-182° C.

後処理

  1. temperatureThe reaction mixture is cooled
  2. filtrationfiltered
  3. customthe filtrate is evaporated under reduced pressure
  4. customto give an oily residue
  5. extractionfrom which 4-hydroxyacetophenone is extracted with ether at pH=1
  6. extractionSubsequent extraction with ethyl acetate at pH=9

出典と根拠

ORDレコード
ord-33222d5c3e74477ea5aecbacd88d0902
出典データセット
uspto-grants-1998_01
特許番号
US05708171

関連ノート

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