Methyl iodide → Methyl 4-fluoro-2-iodo-6-methylbenzoate

HRID 2427725노트

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HRID 2427725 반응식
[F:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:5]([C:6]([OH:8])=[O:7])=[C:4]([I:12])[CH:3]=1.[C:13]([O-])([O-])=O.[K+].[K+].CI>CC(C)=O>[CH3:13][O:7][C:6](=[O:8])[C:5]1[C:9]([CH3:11])=[CH:10][C:2]([F:1])=[CH:3][C:4]=1[I:12]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 672507444-Fluoro-2-iodo-6-methylbenzoic acid

생성물 1

HCID 57949477Methyl 4-fluoro-2-iodo-6-methylbenzoate수율 12%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
70 °C

실험 절차

A solution of 4-fluoro-2-iodo-6-methyl-benzoic acid (8.87 g, 31.8 mmol) in acetone (80 mL) was treated with anhydrous K2CO3 (6.91 g, 50 mmol) followed by methyl iodide (2.72 mL, 40 mmol). The reaction mixture was stirred at 70° C. for 2 h. GC-MS and TLC indicated that the reaction was completed. The solids were removed by filtration and the filtrate evaporated under reduced pressure. Silica gel column chromatography of the resulting material using 10% ethyl acetate in hexanes afforded 4-fluoro-2-iodo-6-methyl-benzoic acid methyl ester (1.1 g, 12%).

후처리

  1. customThe solids were removed by filtration
  2. customthe filtrate evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-068024955a904a2298af04ee0733e863
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968570B2

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