Hydrochloric Acid → Methyl 3-fluoro-4-formylbenzoate

HRID 2233057노트

반응식

HRID 2233057 반응식
[H-].[Na+].[F:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[CH:13]=[O:14])[C:7]([OH:9])=[O:8].[CH3:15]I.Cl>CN(C=O)C>[CH3:15][O:8][C:7](=[O:9])[C:6]1[CH:10]=[CH:11][C:12]([CH:13]=[O:14])=[C:4]([F:3])[CH:5]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 212845583-Fluoro-4-formylbenzoic acid

생성물 1

HCID 18766342Methyl 3-fluoro-4-formylbenzoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

60% NaH (0.14 mol) is added portionwise to a solution of 3-fluoro-4-formyl benzoic acid (3, 0.12 mol) in dry DMF (330 mL). The mixture is stirred at room temperature for 30 min. Methyl iodide (0.14 mol) is added dropwise to the mixture. After stirring at room temperature for 5 h, the reaction mixture is poured into 1 N HCl (ca. 1000 mL) and extracted twice with EtOAc. The combined organic layers are washed with saturated aqueous NaHCO3, brine, dried over MgSO4, and evaporated in vacuo to give crude 3-fluoro-4-formyl benzoic acid methyl ester (4).

후처리

  1. stirringAfter stirring at room temperature for 5 h
  2. extractionextracted twice with EtOAc
  3. washThe combined organic layers are washed with saturated aqueous NaHCO3, brine
  4. dry with materialdried over MgSO4
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-eb3b4645849e44f5a76852583bc8f0ba
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709470B2

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