Diethyl Ether → HCID 22929663, 화합물

HRID 1295954노트

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HRID 1295954 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:14](=[O:16])[CH3:15])[CH:5]=[C:6]([C:10]([CH3:13])([CH3:12])[CH3:11])[C:7]=1[O:8][CH3:9].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].[CH3:25][CH2:26][O:27][CH2:28][CH3:29]>CN(C)C=O.BrOBr>[C:10]([C:6]1[CH:5]=[C:4]([C:14](=[O:16])[CH3:15])[CH:3]=[C:2]([N:1]2[CH2:29][CH2:28][O:27][CH2:26][CH2:25]2)[C:7]=1[O:8][CH3:9])([CH3:11])([CH3:12])[CH3:13]

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 22929815HCID 22929815, 화합물

생성물 1

HCID 22929663HCID 22929663, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 14513628Dibromine monoxide용매

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온도
80 °C

실험 절차

After dissolving 1-[3-amino-5-(tert-butyl)-4-methoxyphenyl]-1-ethanone (180 g) in dimethylformamide (800 ml), dibromoether (125 ml), potassium carbonate (225 g) and sodium iodide (12.2 g) were added and the mixture was stirred at 80° C. for 48 hours. The reaction mixture was cooled to room temperature, 3 l of ether was added and the mixture was washed 3 times with water. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (76 g) as yellow crystals.

후처리

  1. additionwere added
  2. temperatureThe reaction mixture was cooled to room temperature
  3. washthe mixture was washed 3 times with water
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-b0da6e4a1ba24b8c9cd8bd4cc4bb124f
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244730B2

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