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Acetic Acid → HCID 22013889、化合物

HRID 1532747
ノート
印刷プレビュー

反応式

HRID 1532747 の反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][CH2:14][O:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=O)=[CH:18][CH:17]=1.[C:24]([O:33][CH:34]([CH3:36])[CH3:35])(=[O:32])[CH2:25][C:26]([O:28][CH:29]([CH3:31])[CH3:30])=[O:27].C(O)(=O)C.N1CCCCC1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][CH2:14][O:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=[C:25]([C:26]([O:28][CH:29]([CH3:31])[CH3:30])=[O:27])[C:24]([O:33][CH:34]([CH3:36])[CH3:35])=[O:32])=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 8082PiperidineHCID 83223Diisopropyl malonateHCID 107571064-[2-(5-Methyl-2-phenyloxazol-4-yl)ethoxy]benzaldehyde

生成物 1

HCID 22013889HCID 22013889、化合物収率 88%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of 4-[2-(5-methyl-2-phenyl-4-oxazolyl)ethoxy]benzaldehyde (3.07 g, 10 mmol) synthesized according to the method described in WO95/18125 in toluene (40 ml) were added diisopropyl malonate (1.88 g, 10 mmol), acetic acid (300 mg) and piperidine (425 mg). While removing water through Dean-Stark trap, the mixture was refluxed under heating. Eight hours later, toluene was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (developing solvent; hexane:ethyl acetate=75:25) and the fraction containing the objective substance was concentrated under reduced pressure to give the title compound (4.2 g, yield 88%) as a yellow oil.

後処理

  1. customWhile removing water through Dean-Stark trap
  2. temperaturethe mixture was refluxed
  3. temperatureunder heating
  4. customEight hours later, toluene was evaporated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography (developing solvent; hexane:ethyl acetate=75:25)
  6. additionthe fraction containing the objective substance
  7. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-ecfa2bd806f941b0acffa5230ebdfe50
出典データセット
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06204277B1

反応ノート

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