Water → 2-(Morpholin-4-yl)-1,3-thiazole-5-carbaldehyde

HRID 1186375

반응식

HRID 1186375 반응식
Cl[C:2]1[S:3][C:4]([CH:7]=[O:8])=[CH:5][N:6]=1.C(=O)([O-])[O-].[K+].[K+].[NH:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1.O>C(#N)C.C(OCC)(=O)C>[O:18]1[CH2:19][CH2:20][N:15]([C:2]2[S:3][C:4]([CH:7]=[O:8])=[CH:5][N:6]=2)[CH2:16][CH2:17]1

참가 물질

7

반응물 4

HCID 962WaterHCID 8083MorpholineHCID 11430Potassium CarbonateHCID 14797652-Chloro-1,3-thiazole-5-carbaldehyde

생성물 1

HCID 14797702-(Morpholin-4-yl)-1,3-thiazole-5-carbaldehyde수율 66.4%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

2-Chlorothiazole-5-carbaldehyde (200 mg, 1.36 mmol) was dissolved in acetonitrile (4 mL). To this, potassium carbonate (376 mg, 2.72 mmol) and morpholine (0.237 mL, 2.72 mmol) were added at room temperature and the mixture was stirred at the same temperature for 23.5 hours. After water was added to the reaction mixture, extraction with ethyl acetate was performed, followed by washing with brine and drying over anhydrous sodium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by preparative thin-layer chromatography (chloroform/methanol=15/1) to give 2-morpholinothiazole-5-carbaldehyde (179 mg, yield: 66%).

후처리

  1. washby washing with brine
  2. dry with materialdrying over anhydrous sodium sulfate
  3. customThe solvent was evaporated off under reduced pressure
  4. customthe residue was purified by preparative thin-layer chromatography (chloroform/methanol=15/1)

출처 및 근거

ORD 기록
ord-b45d16598c424fb1b190567e53e95327
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08673908B2

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