Methanol → 2-(4-Fluorophenyl)-3-methoxypyrazine

HRID 45566ノート

反応式

HRID 45566 の反応式
Cl[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)=[N:6][CH:5]=[CH:4][N:3]=1.[CH3:15][O-:16].[Na+].CO>O>[F:14][C:11]1[CH:12]=[CH:13][C:8]([C:7]2[C:2]([O:16][CH3:15])=[N:3][CH:4]=[CH:5][N:6]=2)=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 598662582-Chloro-3-(4-fluorophenyl)pyrazine

生成物 1

HCID 598662362-(4-Fluorophenyl)-3-methoxypyrazine収率 96%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Next, 3.87 g of 2-chloro-3-(4-fluorophenyl)pyrazine, 2.01 g of sodium methoxide, and 30 mL of methanol were put in a three-neck flask equipped with a reflux pipe, and reacted by being heated and refluxed under a nitrogen atmosphere for three hours. After the reaction, the reaction solution was cooled down to room temperature, water was added thereto, and an organic layer was extracted with dichloromethane. The obtained organic layer was washed with a saturated saline and water, and dried with magnesium sulfate. Then, magnesium sulfate was removed by filtration and the solvent was distilled off, so that 2-(4-fluorophenyl)-3-methoxypyrazine was obtained (milky white powder, yield: 96%). A synthetic scheme of Step 2 is shown in the following (a1-2).

後処理

  1. customequipped with a reflux pipe
  2. customreacted
  3. temperatureby being heated
  4. temperaturerefluxed under a nitrogen atmosphere for three hours
  5. customAfter the reaction
  6. extractionan organic layer was extracted with dichloromethane
  7. washThe obtained organic layer was washed with a saturated saline and water
  8. dry with materialdried with magnesium sulfate
  9. customThen, magnesium sulfate was removed by filtration
  10. distillationthe solvent was distilled off, so that 2-(4-fluorophenyl)-3-methoxypyrazine
  11. customwas obtained (milky white powder, yield: 96%)

出典と根拠

ORDレコード
ord-dcce1524f3bc4034bb359a74dbbce28f
出典データセット
uspto-grants-2013_09
特許番号
US08541574B2

反応ノート

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