Bromine → 5-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one

HRID 1993345

반응식

HRID 1993345 반응식
[CH3:1][N:2]1[C:7](=[O:8])[CH:6]=[CH:5][N:4]=[C:3]1[S:9][CH3:10].[Br:11]Br>C(Cl)(Cl)Cl>[Br:11][C:6]1[C:7](=[O:8])[N:2]([CH3:1])[C:3]([S:9][CH3:10])=[N:4][CH:5]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 1387273-Methyl-2-(methylthio)-4(3H)-pyrimidinone

생성물 1

HCID 32646665-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
0 °C

실험 절차

3-Methyl-2-methylthio-3H-pyrimidin-4-one (Step 2, 3.31 g, 21.2 mmol) was dissolved in CHCl3 (50 mL) and cooled to 0° C. under Ar. Br2 (1.25 mL, 25.4 mmol) was added via syringe, and the reaction was stirred at 0° C. for 35 min, at which time TLC analysis indicated complete consumption of starting material. The reaction was quenched with 40 mL saturated NaHCO3, warmed to RT, and stirred overnight. The reaction was extracted with CH2Cl2 (3×25 mL), and the organic extracts were combined, dried over Na2SO4, filtered, and concentrated to give the title compound, which did not require further purification. MS (ESI pos. ion) m/z: 236. Calc'd for C6H7BrN2OS: 233.95.

후처리

  1. customconsumption of starting material
  2. customThe reaction was quenched with 40 mL saturated NaHCO3
  3. temperaturewarmed to RT
  4. stirringstirred overnight
  5. extractionThe reaction was extracted with CH2Cl2 (3×25 mL)
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-282f4e6c7edd441e8a0958f1a23ec8c7
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652009B2

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