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Sodium Hydroxide → 2-(p-Pentylphenyl)-5'-propyl-5,2'-bipyrimidinyl

HRID 64586
ノート
印刷プレビュー

反応式

HRID 64586 の反応式
[OH-].[Na+].Cl.[CH2:4]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[N:20]=[CH:19][C:18]([C:21]([NH2:23])=[NH:22])=[CH:17][N:16]=2)=[CH:11][CH:10]=1)[CH2:5][CH2:6][CH2:7][CH3:8]>CO>[CH2:4]([C:9]1[CH:10]=[CH:11][C:12]([C:15]2[N:20]=[CH:19][C:18]([C:21]3[N:23]=[CH:14][C:9]([CH2:4][CH2:5][CH3:6])=[CH:10][N:22]=3)=[CH:17][N:16]=2)=[CH:13][CH:14]=1)[CH2:5][CH2:6][CH2:7][CH3:8]
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 14798Sodium HydroxideHCID 135748272-(p-Pentylphenyl)-5-pyrimidinecarboxamidine hydrochloride

生成物 1

HCID 135748282-(p-Pentylphenyl)-5'-propyl-5,2'-bipyrimidinyl収率 120%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of NaOH (0.8 g, 0.02 mol) dissolved in dry methanol (30 ml) were added 2-(p-pentylphenyl)-5-pyrimidinecarboxamidine hydrochloride (3.0 g, 0.01 mol) and α-propyl -β-dimethylaminoacrolein (1.4 g, 0.01 mol), followed by boiling with stirring for 2 hours and then distilling off methanol. Water (100 ml) and toluene (100 ml) were added to the reaction residue to extract the product, followed by washing the extraction liquor with water, drying the toluene layer over anhydrous sodium sulfate, distilling off toluene and three times recrystallizing the residual solids from ethanol to obtain the objective 2-(p-pentylphenyl)-5'-propyl-5,2'-bipyrimidinyl (2.0 g, 0.006 mol).

後処理

  1. distillationdistilling off methanol
  2. additionWater (100 ml) and toluene (100 ml) were added to the reaction residue
  3. extractionto extract the product
  4. washby washing the extraction liquor with water
  5. dry with materialdrying the toluene layer over anhydrous sodium sulfate
  6. distillationdistilling off toluene and three times
  7. customrecrystallizing the residual solids from ethanol

出典と根拠

ORDレコード
ord-23484c300d70495cb277f2293b4c3a3c
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04609485

反応ノート

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