Methyl iodide → 2-Methoxy-1-nitro-3-(trifluoromethyl)benzene

HRID 501548노트

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HRID 501548 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:13])([F:12])[F:11])[C:5]=1[OH:14])([O-:3])=[O:2].[C:15]([O-])([O-])=O.[K+].[K+].IC>CN(C=O)C>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:11])([F:12])[F:13])[C:5]=1[O:14][CH3:15])([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 9018342-Nitro-6-(trifluoromethyl)phenol

생성물 1

HCID 219358692-Methoxy-1-nitro-3-(trifluoromethyl)benzene수율 92.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
40 °C

실험 절차

To a suspension of compound 17A (1.4 g, 6.76 mmol) and K2CO3 (1.4 g, 10 mmol) in DMF (60 mL) was added iodomethane (0.46 mL, 7.44 mmol). After the addition, the mixture was stirred at 40° C. overnight, then cooled to rt, partitioned between ether and water. The separated ether layer was washed with water and brine, then dried (Na2SO4) and concentrated under reduced pressure. The residue was chromatographed (silica gel) eluting with 10% EtOAc/hexane to yield the title compound (1.38 g, 92% yield).

후처리

  1. additionAfter the addition
  2. temperaturecooled to rt
  3. custompartitioned between ether and water
  4. washThe separated ether layer was washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was chromatographed (silica gel)
  8. washeluting with 10% EtOAc/hexane

출처 및 근거

ORD 기록
ord-de7f567ea8e64129af6501cea2e3c36b
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772267B2

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