Dimethylformamide → 1-[3-(tert-Butyl)-5-(dimethylamino)-4-methoxyphenyl]-1-ethanone

HRID 1295947ノート

反応式

HRID 1295947 の反応式
C(=O)([O-])[O-].[K+].[K+].CI.NC1[CH:11]=[C:12]([C:22](=[O:24])[CH3:23])[CH:13]=[C:14]([C:18]([CH3:21])([CH3:20])[CH3:19])[C:15]=1[O:16][CH3:17].C(OCC)(=O)C.[CH3:31][N:32]([CH3:35])[CH:33]=O>>[C:18]([C:14]1[CH:13]=[C:12]([C:22](=[O:24])[CH3:23])[CH:11]=[C:33]([N:32]([CH3:35])[CH3:31])[C:15]=1[O:16][CH3:17])([CH3:21])([CH3:19])[CH3:20]

参加物

6

反応物 5

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 22929815HCID 22929815、化合物

生成物 1

HCID 589100481-[3-(tert-Butyl)-5-(dimethylamino)-4-methoxyphenyl]-1-ethanone

実験手順

Potassium carbonate (8.5 g, 62 mmol) and methyl iodide (8.8 g, 62 mmol) were added to a solution of 1-[3-amino-5-(tert-butyl)-4-methoxyphenyl]-1-ethanone (6 g, 21 mmol) in dimethylformamide (50 ml) and the mixture was stirred at room temperature for 13 hours. Ethyl acetate was added, the reaction mixture was washed with water and brine in that order and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and then the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (1.9 g) as a light yellow oil.

後処理

  1. washthe reaction mixture was washed with water and brine in that order
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off under reduced pressure
  4. 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-313c1fc3c38c4b4499fc381aff5aafcc
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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