Sodium Hydroxide → HCID 178450079、化合物

HRID 1368553ノート

反応式

HRID 1368553 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([O-])(=O)C.[Na+].Cl.NO.[OH-].[Na+]>C1COCC1.CO>[NH2:14][C:15]1[CH:16]=[C:17]2[C:22](=[CH:23][CH:24]=1)[CH:21]=[C:20]([C:25]([C:30]1[N:31]=[CH:32][NH:33][CH:34]=1)([OH:29])[CH:26]([CH3:28])[CH3:27])[CH:19]=[CH:18]2

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 178450079HCID 178450079、化合物収率 176%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1-{6-[(Diphenylmethylene)amino]naphthalen-2-yl}-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (1.0 g) was dissolved in THF (5 ml)-methanol (5 ml). To the solution were added sodium acetate (285 mg) and hydroxylamine hydrochloride (181 mg), and the mixture was stirred at room temperature for 20 min. To the mixture was added 0.1N-aqueous solution of sodium hydroxide, and the mixture was extracted with ethyl acetate, washed with saturated sodium chloride solution and dried. The solvent was distilled off and the residue was purified by silica gel chromatography (eluent, hexane:ethyl acetate=2:1→1:1) to give the titled compound (720 mg) as a pale red powder.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed with saturated sodium chloride solution
  3. customdried
  4. distillationThe solvent was distilled off
  5. customthe residue was purified by silica gel chromatography (eluent, hexane:ethyl acetate=2:1→1:1)

出典と根拠

ORDレコード
ord-e17d77986f6843d699dd1a551f75dcbe
出典データセット
uspto-grants-2003_06
特許番号
US06573289B1

反応ノート

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