Sodium Hydroxide → N-(3-Allyloxy-4-cyanophenyl)-2,2-dimethylpropionamide

HRID 751052

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HRID 751052 반응식
[CH2:1]([O:4][C:5]1[CH:12]=[C:11]([NH2:13])[CH:10]=[CH:9][C:6]=1[C:7]#[N:8])[CH:2]=[CH2:3].[OH-].[Na+].[C:16](Cl)(=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18]>C(Cl)Cl>[CH2:1]([O:4][C:5]1[CH:12]=[C:11]([NH:13][C:16](=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18])[CH:10]=[CH:9][C:6]=1[C:7]#[N:8])[CH:2]=[CH2:3]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 62493Pivaloyl chlorideHCID 597542362-(Allyloxy)-4-aminobenzonitrile

생성물 1

HCID 59754230N-(3-Allyloxy-4-cyanophenyl)-2,2-dimethylpropionamide수율 92.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

To a solution of 10B (1.9 g, 10.9 mmol) in anhydrous CH2Cl2 (16 mL) cooled at 0° C. was added 1 N aqueous NaOH solution (16.4 mL, 16.4 mmol), followed by pivaloyl chloride (1.9 mL, 15.3 mmol). After the addition, the reaction mixture was stirred at 0° C. for 2 h, then concentrated under reduced pressure to remove most of the CH2Cl2 solvent. The remaining residue was diluted with water, and the resulting precipitate collected by filtration, washed with water, hexane, and dried under vacuum to furnish the title compound as a light brown solid (2.6 g).

후처리

  1. additionAfter the addition
  2. concentrationconcentrated under reduced pressure
  3. customto remove most of the CH2Cl2 solvent
  4. additionThe remaining residue was diluted with water
  5. filtrationthe resulting precipitate collected by filtration
  6. washwashed with water, hexane
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-cdff2f70429e4c22aca803d9dc438fa8
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405234B2

연결된 노트

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