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Water → 1-(4,6-Bis(dimethylamino)pyrimidin-2-yl)piperazine

HRID 1282182
ノート
印刷プレビュー

反応式

HRID 1282182 の反応式
C([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:15]=[C:14]([N:16]([CH3:18])[CH3:17])[CH:13]=[C:12]([N:19]([CH3:21])[CH3:20])[N:11]=2)[CH2:6][CH2:5]1)(=O)C.[OH-].[Na+].O>C(O)C>[CH3:17][N:16]([CH3:18])[C:14]1[CH:13]=[C:12]([N:19]([CH3:20])[CH3:21])[N:11]=[C:10]([N:7]2[CH2:8][CH2:9][NH:4][CH2:5][CH2:6]2)[N:15]=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 962WaterHCID 14798Sodium HydroxideHCID 184231391-Acetyl-4-(4,6-bis(dimethylamino)pyrimidin-2-yl)piperazine

生成物 1

HCID 184231011-(4,6-Bis(dimethylamino)pyrimidin-2-yl)piperazine収率 80.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 1-acetyl-4-(4,6-bis(dimethylamino)pyrimidin-2-yl)piperazine (1.3 g) and sodium hydroxide (0.5 g) in ethanol (15 ml)—water (15 ml) was refluxed under heating for 9.5 hr. The reaction mixture was concentrated under reduced pressure, and ethyl acetate was added to the residue and the mixture was washed with brine. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated to give the title compound (0.9 g) as a pale-brown oil.

後処理

  1. temperatureunder heating for 9.5 hr
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and ethyl acetate
  3. additionwas added to the residue
  4. washthe mixture was washed with brine
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-a1b0cbb35a3a42fca2892d7884be8c98
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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