2-(Methylamino)ethanol → 6-((2-hydroxyethyl)(methyl)amino)pyrimidine-2,4(1H,3H)-dione

HRID 873037노트

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HRID 873037 반응식
[CH3:1][NH:2][CH2:3][CH2:4][OH:5].Cl[C:7]1[NH:12][C:11](=[O:13])[NH:10][C:9](=[O:14])[CH:8]=1>[I-].[K+].O>[OH:5][CH2:4][CH2:3][N:2]([CH3:1])[C:7]1[NH:12][C:11](=[O:13])[NH:10][C:9](=[O:14])[CH:8]=1

참가 물질

5

반응물 2

HCID 80162-(Methylamino)ethanolHCID 732726-Chlorouracil

생성물 1

HCID 867241596-((2-hydroxyethyl)(methyl)amino)pyrimidine-2,4(1H,3H)-dione수율 75.1%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 962Water용매

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온도
120 °C

실험 절차

To a microwave reaction tube 2-(methylamino)ethanol (1.652 g, 22 mmol), 6-chloropyrimidine-2,4(1H,3H)-dione (1.465 g, 10 mmol), potassium iodide (KI) (0.017 g, 0.1 mmol) and water (20 mL) were added. The mixture was heated to 120° C. by microwave (Biotage Initiator) and stirred for 2 h. Then the solution was concentrated in vacuo to remove all the water. EtOH (10 mL) was added to the resultant residue. The suspension was filtered and the filter cake was collected to afford the title compound as a light-yellow solid (1.390 g, 75% yield),

후처리

  1. additionwere added
  2. concentrationThen the solution was concentrated in vacuo
  3. customto remove all the water
  4. additionEtOH (10 mL) was added to the resultant residue
  5. filtrationThe suspension was filtered
  6. customthe filter cake was collected

출처 및 근거

ORD 기록
ord-db23b6ba5cb1450290b0431a9021b412
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975400B2

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