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Potassium Carbonate → HCID 86623130, 화합물

HRID 1926716
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HRID 1926716 반응식
[CH:1]1([C:4]2[N:9]=[CH:8][C:7]([OH:10])=[CH:6][N:5]=2)[CH2:3][CH2:2]1.F[C:12]1[CH:19]=[CH:18][C:15]([CH:16]=[O:17])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[CH:1]1([C:4]2[N:9]=[CH:8][C:7]([O:10][C:12]3[CH:19]=[CH:18][C:15]([CH:16]=[O:17])=[CH:14][CH:13]=3)=[CH:6][N:5]=2)[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 198710372-Cyclopropylpyrimidin-5-ol

생성물 1

HCID 86623130HCID 86623130, 화합물수율 99.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

2-Cyclopropylpyrimidin-5-ol (0.272 g, 2.0 mmol), 4-fluorobenzaldehyde (0.22 mL, 2.1 mmol) and potassium carbonate (0.414 g, 3.0 mmol) in dry DMF (2.0 mL) were heated to 120° C. in a sealed tube for 3 hours. The slurry was diluted with water and extracted twice with EtOAc. The combined organic phases were washed three times with water and brine, dried, filtered and concentrated to give a yellow oil. Purification by column chromatography using 20 g silica and a gradient of 0% to 50% EtOAc-heptanes as eluent gave 0.478 g (99% yield) of the subtitle compound as a colourless oil.

후처리

  1. extractionextracted twice with EtOAc
  2. washThe combined organic phases were washed three times with water and brine
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give a yellow oil
  7. customPurification by column chromatography

출처 및 근거

ORD 기록
ord-c7862ba76660490684ce4124e73f4782
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183251B2

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