Methyl iodide → HCID 178503551, 화합물

HRID 705983

반응식

HRID 705983 반응식
[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

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 7204712-Thiothymine

생성물 1

HCID 178503551HCID 178503551, 화합물수율 71.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-91e9f124d61f4cd9ab6739679d7d8758
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09174968B2

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