Sodium Hydroxide → HCID 178450079, 화합물

HRID 1368553노트

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HRID 1368553 반응식
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

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 22018326HCID 22018326, 화합물

생성물 1

HCID 178450079HCID 178450079, 화합물수율 176%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e17d77986f6843d699dd1a551f75dcbe
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06573289B1

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