Methyl iodide → HCID 178503543, 화합물

HRID 474715

반응식

HRID 474715 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178503543HCID 178503543, 화합물수율 68.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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)

후처리

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

출처 및 근거

ORD 기록
ord-2d3ef4475cc1497cb0978f7424eb30ee
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637536B2

연결된 노트

불러오는 중…