Sodium Hydroxide → HCID 178474043、化合物

HRID 480478ノート

反応式

HRID 480478 の反応式
C1(C(=[N:14][C:15]2[CH:16]=[C:17]3[C:22](=[CH:23][CH:24]=2)[CH:21]=[C:20]([C:25]([C:30]2[N:31]=[CH:32][N:33](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH:34]=2)([OH:29])[CH:26]([CH3:28])[CH3:27])[CH:19]=[CH:18]3)C2C=CC=CC=2)C=CC=CC=1.[C:54]([O-:57])(=O)[CH3:55].[Na+].Cl.NO.[OH-].[Na+]>C1COCC1.CO>[OH:29][C:25]([C:20]1[CH:21]=[C:22]2[C:17](=[CH:18][CH:19]=1)[CH:16]=[C:15]([NH:14][C:54](=[O:57])[CH3:55])[CH:24]=[CH:23]2)([C:30]1[N:31]=[CH:32][NH:33][CH:34]=1)[CH:26]([CH3:27])[CH3:28]

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 22018326HCID 22018326、化合物

生成物 1

HCID 178474043HCID 178474043、化合物収率 164.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 1-{6-[(diphenylmethylene)amino]naphthalene-2-yl}-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (15.0 g) in THF (100 mL)-methanol (100 mL) were added sodium acetate (4.29 g) and hydroxylamine hydrochloride (2.73 g), and the mixture was stirred at room temperature for 20 min. After addition of 0.1N-NaOH solution, the mixture was extracted with ethyl acetate. The extract was washed with brine, dried and concentrated. The residue was dissolved in dichloromethane and pyridine (5.3 mL) and acetic anhydride (4.1 mL) were added. The mixture was stirred at room temperature for 40 min and then saturated sodium bicarbonate solution was added and was extracted with dichloromethane. The extract was dried and concentrated and the residue was crystallized from ethyl acetate to give the titled compound (11.6 g) as pale red crystals.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with brine
  3. customdried
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in dichloromethane
  6. additionpyridine (5.3 mL) and acetic anhydride (4.1 mL) were added
  7. stirringThe mixture was stirred at room temperature for 40 min
  8. additionsaturated sodium bicarbonate solution was added
  9. extractionwas extracted with dichloromethane
  10. customThe extract was dried
  11. concentrationconcentrated
  12. customthe residue was crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-64ac674b98ee4fe693bb4fd5b9eb7c72
出典データセット
uspto-grants-2003_11
特許番号
US06649643B1

反応ノート

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