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Einecs 211-027-4 → CID 117760255

HRID 709610
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HRID 709610 반응식
[CH:1]1([CH:4]([C:11]2[CH:16]=[C:15]([O:17]C)[N:14]=[CH:13][N:12]=2)[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:3][CH2:2]1.[Cl-].[NH+]1C=CC=CC=1.C(=O)([O-])O.[Na+]>CN(C=O)C.C(#N)C>[CH:1]1([CH:4]([C:11]2[CH:16]=[C:15]([OH:17])[N:14]=[CH:13][N:12]=2)[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:3][CH2:2]1
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참가 물질

6

반응물 3

HCID 69401Einecs 211-027-4HCID 516892Sodium BicarbonateHCID 117760142Ethyl 3-cyclopropyl-3-(6-methoxypyrimidin-4-yl)propanoate

생성물 1

HCID 178471101CID 117760255

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6342Acetonitrile용매

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온도
130 °C

실험 절차

Under a nitrogen atmosphere, to a solution of ethyl 3-cyclopropyl-3-(6-methoxypyrimidin-4-yl)propanoate (entire amount) in DMF (15 mL) was added pyridinium chloride (25.9 g), and the mixture was stirred at 130° C. for 20 min. The reaction mixture was cooled to 0° C. and diluted with acetonitrile (20 mL). Sodium hydrogen carbonate (17.0 g) was added to the reaction mixture, the insoluble material was filtered off, and the solvent in the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane), and the obtained solid was washed with diisopropyl ether to give the title compound (3.66 g) as a white solid.

후처리

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. filtrationthe insoluble material was filtered off
  3. customthe solvent in the filtrate was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  5. washthe obtained solid was washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-e6dc28229f74484fa35d70feccfd64c6
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181186B2

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