Methyl iodide → 3-Chloro-5-fluoro-2-methoxybenzaldehyde

HRID 647202노트

반응식

HRID 647202 반응식
[Cl:1][C:2]1[C:3]([OH:11])=[C:4]([CH:7]=[C:8]([F:10])[CH:9]=1)[CH:5]=[O:6].[C:12](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[Cl:1][C:2]1[C:3]([O:11][CH3:12])=[C:4]([CH:7]=[C:8]([F:10])[CH:9]=1)[CH:5]=[O:6]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27827493-Chloro-5-fluoro-2-hydroxybenzaldehyde

생성물 1

HCID 130935603-Chloro-5-fluoro-2-methoxybenzaldehyde수율 69.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

3-Chloro-5-fluoro-2-hydroxybenzaldehyde (2.5 g., 0.014 mole) was taken into 25 ml. of acetone. Potassium carbonate (2.48 g., 0.018 mole) and methyl iodide (2.55 g., 0.018 mole) were added in sequence and the mixture stirred for 16 hours at room temperature. The reaction mixture was filtered and the filtrate concentrated to an oil. The oil was partitioned between methylene chloride and water. The organic layer was washed in sequence with fresh water, 1 N sodium hydroxide and brine, dried over anhydrous magnesium sulfate, and concentrated to yield 3-chloro-5-fluoro-2-methoxybenzaldehyde (1.83 g., 69%; m.p. 59°-62° C.).

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate concentrated to an oil
  3. customThe oil was partitioned between methylene chloride and water
  4. washThe organic layer was washed in sequence with fresh water, 1 N sodium hydroxide and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-52d716b966b345be9568d16dfa910c4f
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04407811

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