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

HRID 873037ノート

反応式

HRID 873037 の反応式
[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

参加物

5

反応物 2

HCID 80162-(Methylamino)ethanolHCID 732726-Chlorouracil

生成物 1

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

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

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),

後処理

  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

出典と根拠

ORDレコード
ord-db23b6ba5cb1450290b0431a9021b412
出典データセット
uspto-grants-2015_03
特許番号
US08975400B2

反応ノート

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