Sodium Hydroxide → [2-Methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-yl]-hydrazine

HRID 2180001노트

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HRID 2180001 반응식
[N:1]([O-])=O.[Na+].[CH3:5][O:6][C:7]1[C:12]([NH2:13])=[CH:11][C:10]([CH3:14])=[C:9]([C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][C:16]=2[O:26][CH3:27])[N:8]=1.Cl[Sn]Cl.[OH-].[Na+]>O.Cl.C(O)(=O)C>[CH3:5][O:6][C:7]1[C:12]([NH:13][NH2:1])=[CH:11][C:10]([CH3:14])=[C:9]([C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:24])([F:25])[F:23])=[CH:17][C:16]=2[O:26][CH3:27])[N:8]=1

참가 물질

8

반응물 4

HCID 14798Sodium HydroxideHCID 24479Stannous ChlorideHCID 224900462-Methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-ylamineHCID 23668193Sodium Nitrite

생성물 1

HCID 22490050[2-Methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-yl]-hydrazine

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매2회HCID 962Water용매2회

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온도
0 °C

실험 절차

A solution of NaNO2 (0.555 g, 8.04 mmol) in water (3 ml) is added to a stirred solution of 2-methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-ylamine (2 g, 6.1 mmol) in concentrated HCl (3 ml), water (3 ml) and acetic acid (8 ml) below 0° C. over 20 minutes. The mixture is added to a stirred solution of SnCl2 2H2O (3.53 g, 15.7 mmol) in 4N HCl (9 ml) at 0° C. over 15 minutes. The mixture is stirred at 0° C. for 20 minutes and at room temperature for 30 minutes. The mixture is basified by NaOH solution at 0° C. and extracted with EtOAc. The combined extracts are dried over Na2SO4 and concentrated under reduced pressure to give [2-methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-yl]-hydrazine. Rf (hexane/EtOAc=1:1)=0.24.

후처리

  1. extractionextracted with EtOAc
  2. dry with materialThe combined extracts are dried over Na2SO4
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9e34bb628fd44de3b5ea867978e83210
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06887875B2

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