Potassium Hydroxide → 5-Bromo-2,4-dimethoxypyridine

HRID 1948240ノート

反応式

HRID 1948240 の反応式
[OH-].[K+].[CH3:3][O:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][N:6]=1.[Br:13]Br>O.[K+].[Br-]>[Br:13][C:8]1[C:9]([O:11][CH3:12])=[CH:10][C:5]([O:4][CH3:3])=[N:6][CH:7]=1

参加物

6

反応物 3

HCID 14797Potassium HydroxideHCID 24408BromineHCID 8177312,4-dimethoxypyridine

生成物 1

HCID 187887085-Bromo-2,4-dimethoxypyridine収率 70%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 253877Potassium Bromide溶媒

実験手順

According to Scheme 23 Step 2: To a solution of KOH (0.5 eq, 0.8 mmol, 40 mg) in water (75 mL) was added 2,4-dimethoxypyridine (1 eq, 2.00 mmol, 0.21 g) followed by the dropwise addition of Br2 (1 eq, 2.00 mmol, 0.20 g) in 1M aqueous KBr solution (75 mL). The reaction was stirred at room temperature for 5 hours and then poured onto water (10 mL) and extracted with CH2Cl2 (3×10 mL). The combined organic fractions were dried (MgSO4), filtered and concentrated under reduced pressure to afford 5-bromo-2,4-dimethoxypyridine (1.40 mmol, 0.30 g, 70%) as a colorless oil. The crude product was reacted on.

後処理

  1. additionpoured onto water (10 mL)
  2. extractionextracted with CH2Cl2 (3×10 mL)
  3. dry with materialThe combined organic fractions were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b916d5ddb70b4b1f919489a5069259ac
出典データセット
uspto-grants-2013_03
特許番号
US08399493B2

反応ノート

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