Methyl iodide → HCID 178503543、化合物

HRID 474715ノート

反応式

HRID 474715 の反応式
[O-][CH2:2]C.[Na+].[N:5]1[CH:10]=[C:9]([CH2:11][C:12]2[C:13](=[O:19])[NH:14][C:15](=[S:18])[NH:16][CH:17]=2)[CH:8]=[N:7][CH:6]=1.CI>CCO>[CH3:2][S:18][C:15]1[NH:16][CH:17]=[C:12]([CH2:11][C:9]2[CH:10]=[N:5][CH:6]=[N:7][CH:8]=2)[C:13](=[O:19])[N:14]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 2723922Sodium ethoxideHCID 109660395-(Pyrimid-5-ylmethyl)-2-thiouracil

生成物 1

HCID 178503543HCID 178503543、化合物収率 68.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Into a stirred solution of sodium ethoxide (157.7 mg, 2.32 mmol, 2 eq) in EtOH (5.2 ml) was added 5-pyrimidin-5-ylmethyl-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (270 mg, 1.22 mmol, 1 eq) at rt. After 30 min, the reaction mixture was treated with methyl iodide (190.7 μl, 3.05 mmol, 2.5 eq) and was stirred at rt overnight. Solvent was evaporated and water (1 ml) was added. pH was adjusted ˜4 with 1N HCl and precipitate was formed to give 2-methylsulfanyl-5-pyrimidin-5-ylmethyl-1H-pyrimidin-4-one (196 mg, yield=62.4%, purity=91%). [M+H]+=235.28. 1H NMR (300 MHz; CDCl3) δ/ppm 2.45 (s, 3H), 3.62 (s, 2H), 3.50 (s, 2H), 7.89 (s, 1H), 8.69 (s, 2H), 9.00 (s, 1H)

後処理

  1. customSolvent was evaporated
  2. additionwater (1 ml) was added
  3. customprecipitate was formed

出典と根拠

ORDレコード
ord-2d3ef4475cc1497cb0978f7424eb30ee
出典データセット
uspto-grants-2014_01
特許番号
US08637536B2

反応ノート

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