Methyl iodide → HCID 178503551、化合物

HRID 474747

反応式

HRID 474747 の反応式
[CH3:1][C:2]1[C:3](=[O:9])[NH:4][C:5](=[S:8])[NH:6][CH:7]=1.[OH-].[K+].[CH3:12]I>C(O)C>[CH3:1][C:2]1[C:3](=[O:9])[N:4]=[C:5]([S:8][CH3:12])[NH:6][CH:7]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 7204712-Thiothymine

生成物 1

HCID 178503551HCID 178503551、化合物収率 71.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5-methyl-2-thiouracil (2 g, 98%, 13.78 mmol, 1 eq) and KOH, 85%, (1.05 eq, 995 mg) were suspended in 25 ml of absolute ethanol and the mixture was stirred for 1 hour at room temperature. In the suspension was then added MeI (1.05 eq, 905 μl) dropwise and the suspension was heated at 65° C. (temperature on display of heating device) for 2 hours. Solvent was then evaporated. In the rest was added 100 ml of water and using ultrasound was suspended. The obtained precipitate was collected by filtration, it was dried and obtained was 5-methyl-2-methylsulfanyl-1H-pyrimidin-4-one (1.7 g, yield=71.9%, purity=93%) in form of a white powder. MS: [M+H]+=157.08 1H NMR (300 MHz; DMSO-d6) δ/ppm 1.90 (s, 3H), 2.50 (s, 3H), 7.78 (s, 1H)

後処理

  1. temperature(temperature on display of heating device) for 2 hours
  2. customSolvent was then evaporated
  3. additionIn the rest was added 100 ml of water
  4. filtrationThe obtained precipitate was collected by filtration, it
  5. customwas dried
  6. customobtained

出典と根拠

ORDレコード
ord-552263b096a04605a0fd7ee7332b43b7
出典データセット
uspto-grants-2014_01
特許番号
US08637536B2

関連ノート

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