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

HRID 1993345

反応式

HRID 1993345 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-282f4e6c7edd441e8a0958f1a23ec8c7
出典データセット
uspto-grants-2010_01
特許番号
US07652009B2

関連ノート

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