Sodium Bicarbonate → HCID 21937990、化合物

HRID 1242199

反応式

HRID 1242199 の反応式
[C:1]1([N:7]2[C:11]3[CH:12]=[C:13]([CH3:16])[CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N+]([O-])([O-])=[O:24].[NH4+].[Ce].C(=O)(O)[O-].[Na+]>S(=O)(=O)(O)O>[C:1]1([N:7]2[C:11]3[CH:12]=[C:13]([CH:16]=[O:24])[CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 130950791,2-diphenyl-6-methyl-1H-benzimidazoleHCID 57418452Ammonium cerium-nitrate

生成物 1

HCID 21937990HCID 21937990、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
80 °C

実験手順

1 g of 1,2-diphenyl-6-methyl-1H-benzimidazole was suspended in 31 ml of 40% sulfuric acid and mixed with 13.5 g of cerium ammonium nitrate. It was allowed to stir for 2.5 hours at 80° C., cooled to 20° C., and carefully stirred into saturated aqueous sodium bicarbonate solution. The mixture was extracted three times with ethyl acetate, the combined extracts were washed with saturated aqueous sodium chloride solution, dried on sodium sulfate solution and evaporated to the dry state in a vacuum. The residue was chromatographed on silica gel.

後処理

  1. temperaturecooled to 20° C.
  2. extractionThe mixture was extracted three times with ethyl acetate
  3. washthe combined extracts were washed with saturated aqueous sodium chloride solution
  4. customdried on sodium sulfate solution
  5. customevaporated to the dry state in a vacuum
  6. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-03cdcc07b1714843a97866c92fc75c34
出典データセット
uspto-grants-2006_10
特許番号
US07115645B2

関連ノート

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