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Formic Acid → 2-(beta-Methoxyethyl)amino-6-(beta-methoxyethyl)aminonitrobenzene

HRID 981821
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HRID 981821 반응식
C.Cl[C:3]1[CH:8]=[C:7]([NH:9][CH2:10][CH2:11][O:12][CH3:13])[C:6]([N+:14]([O-:16])=[O:15])=[C:5]([NH:17][CH2:18][CH2:19][O:20][CH3:21])[CH:4]=1.C(O)=O>C(N(CC)CC)C.O.[Pd]>[CH3:21][O:20][CH2:19][CH2:18][NH:17][C:5]1[CH:4]=[CH:3][CH:8]=[C:7]([NH:9][CH2:10][CH2:11][O:12][CH3:13])[C:6]=1[N+:14]([O-:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 284Formic AcidHCID 297MethaneHCID 200710824-Chloro-2-(beta-methoxyethyl)amino-6-(beta-methoxyethyl)aminonitrobenzene

생성물 1

HCID 200710692-(beta-Methoxyethyl)amino-6-(beta-methoxyethyl)aminonitrobenzene

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 962Water용매
HCID 8471Triethylamine용매

실험 절차

0.4 g of palladium at a concentration of 10% on active charcoal is added to 0.084 mole (25.5 g) of 4-chloro-2-(β-methoxyethyl)amino-6-(β-methoxyethyl)aminonitrobenzene in 33.4 ml of triethylamine, after which 7 ml of formic acid are added dropwise. At the end of the additions, the reaction mixture is heated for 1 hour 30 minutes, under reflux. The reaction mixture is diluted with 100 ml of 96° alcohol and 100 ml of water. The expected product precipitates. After filtration, the expected product containing the catalyst is dissolved in 90 ml of isopropyl alcohol. The catalyst is removed by hot filtration. The expected product crystallizes.

후처리

  1. temperatureAt the end of the additions, the reaction mixture is heated for 1 hour 30 minutes
  2. temperatureunder reflux
  3. customThe expected product precipitates
  4. filtrationAfter filtration
  5. additionthe expected product containing the catalyst
  6. dissolutionis dissolved in 90 ml of isopropyl alcohol
  7. customThe catalyst is removed by hot filtration
  8. customThe expected product crystallizes

출처 및 근거

ORD 기록
ord-abb8d79a029b42918187e3d6971550f6
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04992586

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