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Water → HCID 54291565, 화합물

HRID 1060010
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HRID 1060010 반응식
[H-].[Na+].[CH2:3]([O:5][C:6](=[O:16])[CH2:7]P(OCC)(OCC)=O)[CH3:4].[CH3:17][O:18][C:19]1[CH:24]=[CH:23][N:22]=[C:21]([C:25]2[CH:32]=[CH:31][C:28]([CH:29]=O)=[C:27]([N+:33]([O-:35])=[O:34])[CH:26]=2)[CH:20]=1.O>O1CCCC1>[CH2:3]([O:5][C:6](=[O:16])[CH:7]=[CH:29][C:28]1[CH:31]=[CH:32][C:25]([C:21]2[CH:20]=[C:19]([O:18][CH3:17])[CH:24]=[CH:23][N:22]=2)=[CH:26][C:27]=1[N+:33]([O-:35])=[O:34])[CH3:4]
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참가 물질

6

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HCID 962WaterHCID 13345Triethyl phosphonoacetateHCID 24758Sodium hydrideHCID 186675454-(4-Methoxypyridin-2-yl)-2-nitrobenzaldehyde

생성물 1

HCID 54291565HCID 54291565, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
5 °C

실험 절차

To a suspension of sodium hydride (60% dispersion in mineral oil, 101 mg) in tetrahydrofuran (10 ml) was added a solution of diethylphosphonoacetic acid ethyl ester (0.535 ml) dropwise at 0° C., and the mixture was stirred at 5° C. for 30 minutes. Then to the resultant mixture was added a solution of 4-(4-methoxypyridin-2-yl)-2-nitrobenzaldehyde (543 mg) in tetrahydrofuran (10 ml) dropwise at 0° C., and the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was triturated with diisopropyl ether, filtered and dried to give 4-(4-methoxypyridin-2-yl)-2-nitrocinnamic acid ethyl ester (557 mg).

후처리

  1. stirringthe mixture was stirred at ambient temperature for 1 hour
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue was triturated with diisopropyl ether
  7. filtrationfiltered
  8. customdried

출처 및 근거

ORD 기록
ord-19f6fb3203644195a2d93500a6cad4a5
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06521643B1

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