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Water → n-(4-((4-(4,6-Bis(dimethylamino)-pyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide

HRID 1282183
ノート
印刷プレビュー

反応式

HRID 1282183 の反応式
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=1.[CH3:14][N:15]([CH3:31])[C:16]1[CH:21]=[C:20]([N:22]([CH3:24])[CH3:23])[N:19]=[C:18]([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[N:17]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:23][N:22]([CH3:24])[C:20]1[CH:21]=[C:16]([N:15]([CH3:14])[CH3:31])[N:17]=[C:18]([N:25]2[CH2:30][CH2:29][N:28]([CH2:2][C:3]3[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=3)[CH2:27][CH2:26]2)[N:19]=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 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 15550682N-((4-(chloromethyl)phenyl)methyl)acetamideHCID 184231011-(4,6-Bis(dimethylamino)pyrimidin-2-yl)piperazine

生成物 1

HCID 18423170n-(4-((4-(4,6-Bis(dimethylamino)-pyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide収率 109.8%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A solution of N-(4-chloromethylphenylmethyl)acetamide (0.7 g), 1-(4,6-bis(dimethylamino)pyrimidin-2-yl)piperazine (0.9 g) and potassium carbonate (0.7 g) in dimethylformamide (10 ml) was stirred at 80° C. for 6 hr. The reaction mixture was poured into water (100 ml) and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a brown solid (1.6 g). The obtained brown solid was crystallized from ethyl acetate/ethanol (2:1, 30 ml) to give the title compound (0.9 g) as pale-yellow crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-5df99e7a01f941b0be86b59c7b283d81
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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