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

HRID 598081ノート

反応式

HRID 598081 の反応式
[CH3:1][S:2][C:3]1[NH:8][C:7](=[O:9])[CH:6]=[CH:5][N:4]=1.[Br:10]Br>C(O)(=O)C>[Br:10][C:6]1[C:7](=[O:9])[NH:8][C:3]([S:2][CH3:1])=[N:4][CH:5]=1

参加物

4

反応物 2

HCID 24408BromineHCID 798232-(Methylthio)-1H-pyrimidin-4-one

生成物 1

HCID 2405655-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-one収率 45.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a solution containing 2.0 g (14 mmol) of 2-(methylthio)pyrimidin-4(3H)-one in 10 ml of acetic acid under a nitrogen atmosphere was added 1.04 ml (14 mmol) of bromine in 2 ml acetic acid. The reaction was allowed to stir at room temperature for 30 min. The precipitated product was filtered, washed with acetic acid and suspended in hot acetic acid. To this suspension was added 0.2 ml bromine in 1 ml acetic acid. The product was collected, washed with acetic acid and recrystallized from ethanol to yield 1.4 g (45%) of product.

後処理

  1. filtrationThe precipitated product was filtered
  2. washwashed with acetic acid
  3. additionTo this suspension was added 0.2 ml bromine in 1 ml acetic acid
  4. customThe product was collected
  5. washwashed with acetic acid
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-b4e8dd88e8b74127887858907dba5968
出典データセット
uspto-grants-2011_03
特許番号
US07897607B2

反応ノート

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