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Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester → HCID 70435233, 화합물

HRID 255675
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HRID 255675 반응식
[CH:1]([C:3]1[N:4]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][C:14]=2[CH3:20])[CH:5]=[C:6]([C:10](=[O:12])[CH:11]=1)[C:7]([OH:9])=[O:8])=O.[CH2:21]([O:23][C:24]([CH:26]=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)=[O:25])[CH3:22]>CO>[CH2:21]([O:23][C:24]([CH:26]=[CH:1][C:3]1[N:4]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][C:14]=2[CH3:20])[CH:5]=[C:6]([C:10](=[O:12])[CH:11]=1)[C:7]([OH:9])=[O:8])=[O:25])[CH3:22]
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참가 물질

4

반응물 2

HCID 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl esterHCID 14010769HCID 14010769, 화합물

생성물 1

HCID 70435233HCID 70435233, 화합물수율 32%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 5 ml of methanol was dissolved 0.15 g of 6-formyl-1-(4-hydroxy-2-methylphenyl)-4-oxo-1,4-dihydronicotinic acid, and 0.19 g of ethoxycarbonylmethylenetriphenylphosphorane was added thereto. They were reacted at room temperature for one hour. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and the residue was purified by a column chromatography (Wako Silica Gel C-200; eluent: chloroform/ethanol (50:1 by volume) mixture) to obtain 0.06 g of 6-(2-ethoxycarbonylethenyl)-1-(4-hydroxy-2-methylphenyl)-4-oxo-1,4-dihydronicotinic acid having a melting point of 185°-189° C.

후처리

  1. additionwas added
  2. customThey were reacted at room temperature for one hour
  3. customAfter completion of the reaction
  4. customthe solvent was removed by distillation under reduced pressure
  5. customthe residue was purified by a column chromatography (Wako Silica Gel C-200; eluent: chloroform/ethanol (50:1 by volume) mixture)

출처 및 근거

ORD 기록
ord-da2cec772ee342b1b3e9048c7adbdfcb
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04698352

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