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

HRID 501548

反応式

HRID 501548 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-de7f567ea8e64129af6501cea2e3c36b
出典データセット
uspto-grants-2010_08
特許番号
US07772267B2

関連ノート

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