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Ethanol → Tert-butyl 8-amino-2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate

HRID 2070124
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HRID 2070124 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:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:5]2.C(O)C.C([O-])=O.[NH4+]>[Pd].O1CCCC1>[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:23])[O:18][C:19]([CH3:21])([CH3:20])[CH3:22])[CH2:5]2
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참가 물질

6

반응물 3

HCID 702EthanolHCID 2723923Ammonium formateHCID 59620339Tert-butyl 6-bromo-8-nitro-2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate

생성물 1

HCID 59620337Tert-butyl 8-amino-2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate수율 92.7%

시약·촉매·용매 2

HCID 23938Palladium촉매
HCID 8028
Tetrahydrofuran
용매

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온도
65 °C

실험 절차

tert-Butyl 6-bromo-8-nitro-2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate (628 g) was added to ethanol (3.1 L), and the mixture was heated at 65° C. To the mixture, 10% Pd—C (water content: 53%) (67.1 g) and ammonium formate (1.03 kg) were sequentially added, and the resultant mixture was stirred for 10 minutes under heating and reflux. Tetrahydrofuran (2.5 L) was added to the reaction mixture so as to dissolve the precipitates, and undissolved matter was removed through filtration with Celite. The filtrate was concentrated under reduced pressure, and water was added to the residue. The formed precipitates were recovered through filtration. The thus-obtained solid was dried, whereby the title compound (418 g) was yielded as a powdery compound.

후처리

  1. temperatureunder heating
  2. temperaturereflux
  3. dissolutionto dissolve the precipitates, and undissolved matter
  4. customwas removed through filtration with Celite
  5. concentrationThe filtrate was concentrated under reduced pressure, and water
  6. additionwas added to the residue
  7. customThe formed precipitates
  8. filtrationwere recovered through filtration
  9. customThe thus-obtained solid was dried

출처 및 근거

ORD 기록
ord-dff2b37bf64c47afbde109e71214a0d8
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299255B2

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