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

HRID 64586
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HRID 64586 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 135748272-(p-Pentylphenyl)-5-pyrimidinecarboxamidine hydrochloride

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-23484c300d70495cb277f2293b4c3a3c
출처 데이터셋
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04609485

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