Methyl iodide → Methyl 3-iodo-4-methyl-5-nitrobenzoate

HRID 59800

반응식

HRID 59800 반응식
[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].[C:15]([O-])([O-])=O.[K+].[K+].CI>CC(C)=O>[CH3:15][O:6][C:5](=[O:7])[C:4]1[CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]([CH3:11])=[C:2]([I:1])[CH:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 596277773-Iodo-4-methyl-5-nitrobenzoic acid

생성물 1

HCID 24728110Methyl 3-iodo-4-methyl-5-nitrobenzoate수율 98.3%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
40 °C

실험 절차

To a solution of 3-iodo-4-methyl-5-nitro-benzoic acid (16.06 g, 52.3 mmol) in acetone (300 mL) was added K2CO3 (14.46 g, 104.6 mmol) followed by methyl iodide ((3.91 mL, 62.76 mmol). The reaction mixture was stirred at 40° C. overnight, then cooled to room temperature and partitioned between ethyl acetate and brine. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to provide 16.5 g (98%) of 3-iodo-4-methyl-5-nitro-benzoic acid methyl ester.

후처리

  1. temperaturecooled to room temperature
  2. custompartitioned between ethyl acetate and brine
  3. customThe organic layer was separated
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-821743cb204d42a1a8a745aa8aed2a07
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440956B2

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