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4-[1-(3-Nitro-2-pyridyl)piperazin-4-yl-carbonyl]benzoic acid methyl ester → HCID 11110580、化合物

HRID 582292
ノート
印刷プレビュー

反応式

HRID 582292 の反応式
[CH3:1][O:2][C:3](=[O:27])[C:4]1[CH:9]=[CH:8][C:7]([C:10]([N:12]2[CH2:17][CH2:16][N:15]([C:18]3[C:23]([N+:24]([O-])=O)=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:14][CH2:13]2)=[O:11])=[CH:6][CH:5]=1.[H][H]>CO.C(Cl)Cl.[Ni]>[CH3:1][O:2][C:3](=[O:27])[C:4]1[CH:9]=[CH:8][C:7]([C:10]([N:12]2[CH2:13][CH2:14][N:15]([C:18]3[C:23]([NH2:24])=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:16][CH2:17]2)=[O:11])=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 118107654-[1-(3-Nitro-2-pyridyl)piperazin-4-yl-carbonyl]benzoic acid methyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 11110580HCID 11110580、化合物収率 88.1%

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 887Methanol溶媒HCID 6344Dichloromethane
溶媒

実験手順

4-[1-(3-Nitro-2-pyridyl)piperazin-4-yl-carbonyl]benzoic acid methyl ester (5 g) was dissolved in a co-solvent of methanol (80 ml) and methylene chloride (60 ml) in a pressurized reactor. With the addition of about 1 g of Raney-nickel (50% slurry in water), the reaction mixture was filled with hydrogen gas and stirred at 50~60 psi for 4 hours. After completion of the reaction, reaction mixture was filtered through celite and filtrate was concentrated under reduced pressure. The concentrated residue was treated with hexane and ether for crystallization, filtered, washed and dried to give 4.05 g (yield: 88%) of the desired compound.

後処理

  1. customAfter completion of the reaction, reaction mixture
  2. filtrationwas filtered through celite and filtrate
  3. concentrationwas concentrated under reduced pressure
  4. additionThe concentrated residue was treated with hexane and ether for crystallization
  5. filtrationfiltered
  6. washwashed
  7. customdried

出典と根拠

ORDレコード
ord-9ba848712bfb4feda5b206c85dda0741
出典データセット
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05922871

反応ノート

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