Diethyl Ether → HCID 22929663、化合物

HRID 1295954ノート

反応式

HRID 1295954 の反応式
[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]

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 22929815HCID 22929815、化合物

生成物 1

HCID 22929663HCID 22929663、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 14513628Dibromine monoxide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b0da6e4a1ba24b8c9cd8bd4cc4bb124f
出典データセット
uspto-grants-2007_07
特許番号
US07244730B2

反応ノート

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