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1-(2-Hydroxyethyl)piperazine → Acetamide, N-(8-(4-(2-hydroxyethyl)-1-piperazinyl)-1,7-naphthyridin-6-yl)-

HRID 542715
ノート
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反応式

HRID 542715 の反応式
[C:1]([NH:4][C:5]1[CH:6]=[C:7]2[C:12](=[C:13](Br)[N:14]=1)[N:11]=[CH:10][CH:9]=[CH:8]2)(=[O:3])[CH3:2].[N:16]1([CH2:22][CH2:23][OH:24])[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>C(OC(O)C)C>[C:1]([NH:4][C:5]1[CH:6]=[C:7]2[C:12](=[C:13]([N:19]3[CH2:20][CH2:21][N:16]([CH2:22][CH2:23][OH:24])[CH2:17][CH2:18]3)[N:14]=1)[N:11]=[CH:10][CH:9]=[CH:8]2)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 76771-(2-Hydroxyethyl)piperazineHCID 138267326-Acetamido-8-bromo-1,7-naphthyridine

生成物 1

HCID 3065021Acetamide, N-(8-(4-(2-hydroxyethyl)-1-piperazinyl)-1,7-naphthyridin-6-yl)-収率 82.5%

試薬・触媒・溶媒 1

HCID 101298981-Ethoxyethanol溶媒2 回

実験手順

To a mixture of 2.66 g of 6-acetamido-8-bromo-1,7-naphthyridine and 6.51 g of 1-piperazine ethanol, 180 ml of ethoxyethanol was added. The resultant mixture was refluxed with stirring for 45 minutes. After the reaction, ethoxyethanol was distilled off under reduced pressure and chloroform was added to the residue. After thoroughly washing the chloroform solution with water, it was dried with anhydrous magnesium sulfate. Chloroform was distilled off under reduced pressure and the residue was purified by silica gel column chromatography, followed by recrystallization from a mixed solvent of ethanol and ether to obtain 2.6 g of 6-acetamido-8-[4-(2-hydroxyethyl)-1-piperazinyl]-1,7-naphthyridine (Compound No. 22) as light yellowish crystals (yield: 82.5%).

後処理

  1. additionwas added
  2. distillationwas distilled off under reduced pressure and chloroform
  3. additionwas added to the residue
  4. washAfter thoroughly washing the chloroform solution with water, it
  5. dry with materialwas dried with anhydrous magnesium sulfate
  6. distillationChloroform was distilled off under reduced pressure
  7. customthe residue was purified by silica gel column chromatography
  8. customfollowed by recrystallization from a mixed solvent of ethanol and ether

出典と根拠

ORDレコード
ord-8d40f003db9c421ebb918910e3a30b1c
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04659710

反応ノート

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