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

HRID 501532ノート

反応式

HRID 501532 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0be4df673f34498a9fada774b89f347a
出典データセット
uspto-grants-2010_08
特許番号
US07772267B2

反応ノート

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