Lithium Hydroxide → 6-Chloro-4-(2-fluoro-4-nitrobenzyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridine

HRID 2240218노트

반응식

HRID 2240218 반응식
[Cl:1][C:2]1[N:7]=[C:6]2[N:8]([CH2:11][O:12][CH2:13][CH2:14][Si:15]([CH3:18])([CH3:17])[CH3:16])[CH:9]=[CH:10][C:5]2=[C:4]([CH:19]([C:24]2[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][C:25]=2[F:33])C(OC)=O)[CH:3]=1.[OH-].[Li+]>CO.O>[Cl:1][C:2]1[N:7]=[C:6]2[N:8]([CH2:11][O:12][CH2:13][CH2:14][Si:15]([CH3:17])([CH3:18])[CH3:16])[CH:9]=[CH:10][C:5]2=[C:4]([CH2:19][C:24]2[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][C:25]=2[F:33])[CH:3]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 59304979HCID 59304979, 화합물

생성물 1

HCID 593050056-Chloro-4-(2-fluoro-4-nitrobenzyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridine

시약·촉매·용매 2

HCID 962Water촉매HCID 887Methanol용매

실험 절차

358 mg (0.72 mmol) of methyl (6-chloro-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)(2-fluoro-4-nitrophenyl)acetate are dissolved in 6 ml of methanol. 21 mg (0.87 mmol) of lithium hydroxide and 2 drops of water are added, and the mixture is stirred at RT for 20 hours. The mixture is concentrated under reduced pressure, dichloromethane and water are added and the organic phase is separated off and dried over sodium sulfate. The solvent is removed under reduced pressure and the product is purified by chromatography on silica gel (mobile phase: dichloromethane). This gives an oil.

후처리

  1. concentrationThe mixture is concentrated under reduced pressure, dichloromethane and water
  2. additionare added
  3. customthe organic phase is separated off
  4. dry with materialdried over sodium sulfate
  5. customThe solvent is removed under reduced pressure
  6. customthe product is purified by chromatography on silica gel (mobile phase: dichloromethane)
  7. customThis gives an oil

출처 및 근거

ORD 기록
ord-18c7ba106e9b450d92f075b282fc6ae6
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723347B2

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