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Triethylamine → N-(4-((4-(pyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)propionamide

HRID 1282135
ノート
印刷プレビュー

反応式

HRID 1282135 の反応式
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16]3[N:21]=[CH:20][CH:19]=[CH:18][N:17]=3)[CH2:12][CH2:11]2)=[CH:5][CH:4]=1.[C:22](Cl)(=[O:25])[CH2:23][CH3:24].C(N(CC)CC)C>C(Cl)Cl>[N:21]1[CH:20]=[CH:19][CH:18]=[N:17][C:16]=1[N:13]1[CH2:12][CH2:11][N:10]([CH2:9][C:6]2[CH:7]=[CH:8][C:3]([CH2:2][NH:1][C:22](=[O:25])[CH2:23][CH3:24])=[CH:4][CH:5]=2)[CH2:15][CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 184230082-(4-(4-(Aminomethyl)phenylmethyl)piperazin-1-yl)pyrimidine

生成物 1

HCID 18423155N-(4-((4-(pyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)propionamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 2-(4-(4-(aminomethyl)phenylmethyl)piperazin-1-yl)pyrimidine (0.5 g), propionic chloride (0.18 ml) and triethylamine (0.3 ml) in methylene chloride (20 ml) was stirred at room temperature for 2 hr. The reaction mixture was washed with water and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give a pale-yellow substance (0.8 g). The obtained pale-yellow substance was crystallized from hexane/ethyl acetate (1:1, 50 ml) to give the title compound (0.5 g) as pale-yellow crystals.

後処理

  1. washThe reaction mixture was washed with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customto give a pale-yellow substance (0.8 g)
  5. customThe obtained pale-yellow substance was crystallized from hexane/ethyl acetate (1:1, 50 ml)

出典と根拠

ORDレコード
ord-6364f0b9980148818ad4fcac88e24980
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06455528B1

反応ノート

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