Sodium Bicarbonate → HCID 178474043、化合物

HRID 392586ノート

反応式

HRID 392586 の反応式
[OH:1][C:2]([C:30]1[CH:31]=[C:32]2[C:37](=[CH:38][CH:39]=1)[CH:36]=[C:35]([NH:40][C:41](=[O:43])[CH3:42])[CH:34]=[CH:33]2)([C:6]1[N:7]=[CH:8][N:9](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:10]=1)[CH:3]([CH3:5])[CH3:4].Cl.N1C=CC=CC=1.C(=O)([O-])O.[Na+]>CO>[OH:1][C:2]([C:30]1[CH:31]=[C:32]2[C:37](=[CH:38][CH:39]=1)[CH:36]=[C:35]([NH:40][C:41](=[O:43])[CH3:42])[CH:34]=[CH:33]2)([C:6]1[N:7]=[CH:8][NH:9][CH:10]=1)[CH:3]([CH3:5])[CH3:4]

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 10176127Pyridinium chlorideHCID 22018433HCID 22018433、化合物

生成物 1

HCID 178474043HCID 178474043、化合物収率 84%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

N-{6-[1-Hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]naphthalen-2-yl}acetamide (11.5 g) and pyridine hydrochloride (390 mg) were dissolved in methanol (8 ml) and the mixture was stirred at 60° C. for 2 h. After allowing to cool, the mixture was neutralized with saturated aqueous sodium hydrogen carbonate. The solvent was evaporated and the residue was collected by filtration and washed with ethanol. The filtrate was concentrated and the obtained residue was purified by silica gel column chromatography (eluate, dichloromethane:methanol =30:1→10:1) and recrystallized from ethyl acetate to give the title compound (5.52 g) as a pale-red powder.

後処理

  1. temperatureto cool
  2. customThe solvent was evaporated
  3. filtrationthe residue was collected by filtration
  4. washwashed with ethanol
  5. concentrationThe filtrate was concentrated
  6. customthe obtained residue was purified by silica gel column chromatography (eluate, dichloromethane:methanol =30:1→10:1)
  7. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-1cd844a03f744ff7be025c69766b4d69
出典データセット
uspto-grants-2004_10
特許番号
US06800778B1

反応ノート

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