Potassium Carbonate → HCID 59643238, 화합물

HRID 2251539노트

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HRID 2251539 반응식
[CH3:1][C:2]([O:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][NH:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=2)=[CH:12][CH:11]=1)([CH3:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl[C:31]1[CH:36]=[CH:35][C:34]([N+:37]([O-:39])=[O:38])=[CH:33][N:32]=1.C([O-])([O-])=O.[K+].[K+]>O1CCOCC1>[CH3:8][C:2]([O:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][N:18]([C:31]2[CH:36]=[CH:35][C:34]([N+:37]([O-:39])=[O:38])=[CH:33][N:32]=2)[CH2:19][C:20]2[CH:21]=[CH:22][C:23]([C:26]([F:27])([F:28])[F:29])=[CH:24][CH:25]=2)=[CH:12][CH:11]=1)([CH3:1])[C:3]([O:5][CH2:6][CH3:7])=[O:4]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 783082-Chloro-5-nitropyridineHCID 59643115HCID 59643115, 화합물

생성물 1

HCID 59643238HCID 59643238, 화합물수율 78.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of ethyl 2-methyl-2-[4-(2-{[4-(trifluoromethyl)benzyl]amino}ethyl)phenoxy]propanoate (250 mg; 0.61 mmol), 2-chloro-5-nitro-pyridine (116 mg; 0.73 mmol) and K2CO3 (126 mg; 0.92 mmol) in 2 ml of dioxane was heated at 220C in a pressure tube under nitrogen for 16 hr. Upon cooling, the mixture was partitioned between ethyl acetate and water. The aqueous phase was washed with ethyl acetate and the combined organic phases were washed with brine, dried over sodium sulfate and concentrated. Purification by radial chromatography using ethyl acetate-hexane mixtures (2–30% gradient) afforded the title compound (254 mg; 78% yield).

후처리

  1. temperatureUpon cooling
  2. customthe mixture was partitioned between ethyl acetate and water
  3. washThe aqueous phase was washed with ethyl acetate
  4. washthe combined organic phases were washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customPurification by radial chromatography

출처 및 근거

ORD 기록
ord-89e07f800706492da910ada71f48b0de
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07319104B2

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