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

HRID 2922

반응식

HRID 2922 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
0 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-008f672ce81f498d931758715cd6380b
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731340

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