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

HRID 981821
ノート
印刷プレビュー

反応式

HRID 981821 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 962Water溶媒
HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-abb8d79a029b42918187e3d6971550f6
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04992586

反応ノート

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