Ethyl Acetate → HCID 21894663、化合物

HRID 1242916ノート

反応式

HRID 1242916 の反応式
[N+:1]([C:4]1[CH:5]=[N:6][C:7]2[CH2:8][CH2:9][CH2:10][CH2:11][C:12]=2[CH:13]=1)([O-])=O.[C:14](OCC)(=[O:16])[CH3:15]>[C].[Pd].CO>[N:6]1[C:7]2[CH2:8][CH2:9][CH2:10][CH2:11][C:12]=2[CH:13]=[C:4]([NH:1][C:14](=[O:16])[CH3:15])[CH:5]=1

参加物

5

反応物 2

HCID 8857Ethyl AcetateHCID 110303733-nitro-5,6,7,8-tetrahydroquinoline

生成物 1

HCID 21894663HCID 21894663、化合物

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

10% Palladium-carbon (200 mg) was added to a methanol solution (68 ml) of 3-nitro-5,6,7,8-tetrahydroquinoline (2.41 g], 13.5 mmol) obtained in 2), which was stirred under hydrogen atmosphere for 16 hours. After a catalyst was filtered off, the solvent was distilled out under reduced pressure. The resulting residue was dissolved in pyridine (35 ml). Anhydrous ethyl acetate (1.91 ml, 20.3 mmol) was added to the solution, which was stirred at room temperature for 1 hour. After completion of the reaction, the solvent was distilled out under reduced pressure. Diisopropyl ether-n-hexane (1:8) was added to the resulting residue, to give the titled compound (2.48 g) as a colorless powder.

後処理

  1. customobtained in 2), which
  2. filtrationAfter a catalyst was filtered off
  3. distillationthe solvent was distilled out under reduced pressure
  4. dissolutionThe resulting residue was dissolved in pyridine (35 ml)
  5. stirringwas stirred at room temperature for 1 hour
  6. customAfter completion of the reaction
  7. distillationthe solvent was distilled out under reduced pressure
  8. additionDiisopropyl ether-n-hexane (1:8) was added to the resulting residue

出典と根拠

ORDレコード
ord-d2530d02b18e46409dac244a5ac42687
出典データセット
uspto-grants-2006_10
特許番号
US07115750B1

反応ノート

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