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Ethanol → HCID 9846356、化合物

HRID 1938342
ノート
印刷プレビュー

反応式

HRID 1938342 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][O:14][C:15]1[CH:24]=[C:23]2[C:18]([CH:19]=[C:20]([CH2:25][CH:26]3[S:30][C:29](=N)[NH:28][C:27]3=[O:32])[CH:21]=[N:22]2)=[CH:17][CH:16]=1.C([OH:35])C>Cl>[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][O:14][C:15]1[CH:24]=[C:23]2[C:18]([CH:19]=[C:20]([CH2:25][CH:26]3[S:30][C:29](=[O:35])[NH:28][C:27]3=[O:32])[CH:21]=[N:22]2)=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 702EthanolHCID 140385021HCID 140385021、化合物

生成物 1

HCID 9846356HCID 9846356、化合物収率 11%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

In a mixture of 3N hydrochloric acid (4 mL) and ethanol (2 mL) was dissolved 5-[[7-(5-methyl-2-phenyl-4-oxazolylmethoxy)-3-quinolyl]methyl]-2-iminothiazolidin-4-one (100 mg, 0.22 mmol.). The resulting solution was heated under reflux for 12 hours. After the completion of reaction was confirmed, ethanol was distilled off. To the residue were added ethyl acetate and aqueous sodium hydrogen carbonate. The organic portion was recovered, washed with water, and dried over sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/3), to give 11 mg of the desired compound as pale brown crystalline powder (yield 11%).

後処理

  1. temperatureThe resulting solution was heated
  2. temperatureunder reflux for 12 hours
  3. customAfter the completion of reaction
  4. distillationethanol was distilled off
  5. additionTo the residue were added ethyl acetate and aqueous sodium hydrogen carbonate
  6. customThe organic portion was recovered
  7. washwashed with water
  8. dry with materialdried over sodium sulfate
  9. distillationThe solvent was distilled off under reduced pressure
  10. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/3)

出典と根拠

ORDレコード
ord-0ad267cc8b2c4946926d83cb1dd63dda
出典データセット
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05693651

反応ノート

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