Water → HCID 59620340, 화합물

HRID 2070146노트

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HRID 2070146 반응식
Br[C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([N+:12]([O-])=O)[CH:11]=1)[NH:8][C:7](=[O:15])[CH:6]([NH:16][C:17](=[O:19])[CH3:18])[CH2:5]2.C([O-])=O.[NH4+].O>C(O)C.[Pd]>[NH2:12][C:10]1[CH:11]=[CH:2][CH:3]=[C:4]2[C:9]=1[NH:8][C:7](=[O:15])[CH:6]([NH:16][C:17](=[O:19])[CH3:18])[CH2:5]2

참가 물질

6

반응물 3

HCID 962WaterHCID 2723923Ammonium formateHCID 59620398HCID 59620398, 화합물

생성물 1

HCID 59620340HCID 59620340, 화합물수율 84.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매2회

반응 조건

온도
80 °C

실험 절차

N-(6-Bromo-8-nitro-2-oxo-1,2,3,4-tetrahydroquinolin-3-yl)acetamide (15 g) was suspended in ethanol (150 mL), and ammonium formate (28.8 g) and 10% Pd—C (water content: 53%) (1.5 g) were added thereto. The mixture was heated at 80° C. while being stirred for 30 minutes, and water (150 mL) and ethanol (150 mL) were added thereto, followed by filtration while being heated. The filtrate was concentrated under reduced pressure, and the formed precipitates were recovered through filtration. The thus-obtained solid was washed with ethanol and diisopropyl ether, followed by drying, whereby the title compound (8.5 g) was yielded.

후처리

  1. filtrationfollowed by filtration
  2. temperaturewhile being heated
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe formed precipitates
  5. filtrationwere recovered through filtration
  6. washThe thus-obtained solid was washed with ethanol and diisopropyl ether
  7. customby drying

출처 및 근거

ORD 기록
ord-058ec640b9c144c283f449fb6605c12c
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299255B2

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