Water → N-[2-methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-yl]-N-propyl-propionamide

HRID 1354245노트

반응식

HRID 1354245 반응식
[H-].[Na+].[CH3:3][O:4][C:5]1[C:10]([NH:11][C:12](=[O:15])[CH2:13][CH3:14])=[CH:9][C:8]([CH3:16])=[C:7]([C:17]2[CH:22]=[CH:21][C:20]([O:23][C:24]([F:27])([F:26])[F:25])=[CH:19][C:18]=2[O:28][CH3:29])[N:6]=1.I[CH2:31][CH2:32][CH3:33].O>CN(C=O)C>[CH3:3][O:4][C:5]1[C:10]([N:11]([CH2:31][CH2:32][CH3:33])[C:12](=[O:15])[CH2:13][CH3:14])=[CH:9][C:8]([CH3:16])=[C:7]([C:17]2[CH:22]=[CH:21][C:20]([O:23][C:24]([F:27])([F:26])[F:25])=[CH:19][C:18]=2[O:28][CH3:29])[N:6]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 336431-IodopropaneHCID 21104864N-[2-methoxy-6-(2-methoxy-4-trifluoromethoxyphenyl)-5-methyl-pyridin-3-yl]-propionamide

생성물 1

HCID 21104863N-[2-methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-yl]-N-propyl-propionamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

60% NaH (23 mg, 0.58 mmol) is added to a solution of N-[2-methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-yl]-propionamide (0.15 g, 0.39 mmol) in DMF (1 ml) at room temperature. After stirring at room temperature for 20 minutes, iodo propane (0.058 ml, 0.58 mmol) is added. The mixture is stirred at room temperature for 3 days. 20 ml of water is added and the mixture is extracted with EtOAc. The combined extracts are washed with brine and dried over Na2SO4. The solvent is removed under reduced pressure and the residue is purified by flash column chromatography to give N-[2-methoxy-6-(2-methoxy-4-trifluoromethoxy-phenyl)-5-methyl-pyridin-3-yl]-N-propyl-propionamide. Rf (hexane/EtOAc=2:1)=0.42.

후처리

  1. stirringThe mixture is stirred at room temperature for 3 days
  2. extractionthe mixture is extracted with EtOAc
  3. washThe combined extracts are washed with brine
  4. dry with materialdried over Na2SO4
  5. customThe solvent is removed under reduced pressure
  6. customthe residue is purified by flash column chromatography

출처 및 근거

ORD 기록
ord-f8280af0d3a14ae1b2279362db9ff73a
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223778B2

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