Sodium Cyanide → 2-(2-tert-Butyl-1,3-oxazol-4-yl)acetonitrile

HRID 1107690ノート

反応式

HRID 1107690 の反応式
[C-:1]#[N:2].[Na+].[C:4]([C:8]1[O:9][CH:10]=[C:11]([CH2:13]Cl)[N:12]=1)([CH3:7])([CH3:6])[CH3:5].[OH-].[Na+]>CS(C)=O>[C:4]([C:8]1[O:9][CH:10]=[C:11]([CH2:13][C:1]#[N:2])[N:12]=1)([CH3:7])([CH3:6])[CH3:5]

参加物

5

反応物 3

HCID 8929Sodium CyanideHCID 14798Sodium HydroxideHCID 221695102-tert-Butyl-4-(chloromethyl)-1,3-oxazole

生成物 1

HCID 221695172-(2-tert-Butyl-1,3-oxazol-4-yl)acetonitrile収率 92.6%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

反応条件

温度
65 °C

実験手順

6.2 g of sodium cyanide was weighed, 50 ml of dimethylsulfoxide was added thereto, and a dimethylsulfoxide solution of 16.9 g of 2-tert-butyl-4-chloromethyloxazole was dropwise added thereto, and heated on an oil bath at 65° C. for 1 hour with stirring. After the resulting product was cooled to room temperature, 150 ml of a dilute aqueous solution of sodium hydroxide was added thereto, and extracted with toluene. The organic layer was fully washed with water, and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to obtain 14.8 g of 2-tert-butyl-4-cyanomethyloxazole.

後処理

  1. temperatureAfter the resulting product was cooled to room temperature
  2. extractionextracted with toluene
  3. washThe organic layer was fully washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-d61ed4083b1b451c9bf8c1987ba919e5
出典データセット
uspto-grants-2000_05
特許番号
US06063734

反応ノート

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