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

HRID 1948240노트

반응식

HRID 1948240 반응식
[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

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 24408BromineHCID 8177312,4-dimethoxypyridine

생성물 1

HCID 187887085-Bromo-2,4-dimethoxypyridine수율 70%

시약·촉매·용매 2

HCID 962Water용매HCID 253877Potassium Bromide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b916d5ddb70b4b1f919489a5069259ac
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399493B2

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