Water → N-(2,6-dimethoxy-4-methylphenyl)isovaleramide

HRID 2922

反応式

HRID 2922 の反応式
[CH3:1][O:2][C:3]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([O:11][CH3:12])[C:4]=1[NH2:5].C(N(CC)CC)C.[C:20](Cl)(=[O:25])[CH2:21][CH:22]([CH3:24])[CH3:23].O>C(OCC)C>[CH3:12][O:11][C:6]1[CH:7]=[C:8]([CH3:10])[CH:9]=[C:3]([O:2][CH3:1])[C:4]=1[NH:5][C:20](=[O:25])[CH2:21][CH:22]([CH3:24])[CH3:23]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 66054Isovaleryl chlorideHCID 124090902,6-Dimethoxy-4-methylaniline

生成物 1

HCID 18936492N-(2,6-dimethoxy-4-methylphenyl)isovaleramide収率 92%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

8.2 g of 2,6-dimethoxy-4-methylaniline are dissolved in 100 ml of diethyl ether at 0° C. under an inert atmosphere, 5.96 g of triethylamine are added to the reaction mixture and then 6.51 g of isovaleryl chloride are added dropwise, while maintaining the temperature at 0° C. The mixture is left at room temperature for 30 minutes and is then poured into 250 ml of water. The aqueous phase is extracted with ethyl acetate after separation by settling of the ethereal phase. The organic phases are combined and washed with water, then dried over anhydrous sodium sulphate and evaporated to dryness. The white crystals of N-(2,6-dimethoxy-4-methylphenyl)isovaleramide obtained are washed with diisopropyl ether; M.p.=139° C., Yield: 92%.

後処理

  1. additionare added to the reaction mixture
  2. extractionThe aqueous phase is extracted with ethyl acetate
  3. customafter separation
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulphate
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-008f672ce81f498d931758715cd6380b
出典データセット
uspto-grants-1998_03
特許番号
US05731340

関連ノート

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