Ethyl Acetate → HCID 21894663, 화합물

HRID 1242916노트

반응식

HRID 1242916 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 21894663HCID 21894663, 화합물

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d2530d02b18e46409dac244a5ac42687
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07115750B1

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