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Allyl chloride → alpha-Allyl-alpha-isopropyl-2-methylbenzyl cyanide

HRID 21815
ノート
印刷プレビュー

反応式

HRID 21815 の反応式
[OH-].[Na+].[CH:3]([CH:6]([C:14]#[N:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH3:13])([CH3:5])[CH3:4].[CH2:16](Cl)[CH:17]=[CH2:18]>O.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:18]([C:6]([C:14]#[N:15])([CH:3]([CH3:5])[CH3:4])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH3:13])[CH:17]=[CH2:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7850Allyl chlorideHCID 14798Sodium HydroxideHCID 142451303-Methyl-2-(2-methylphenyl)butanenitrile

生成物 1

HCID 19933531alpha-Allyl-alpha-isopropyl-2-methylbenzyl cyanide収率 93%

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 962
Water
溶媒
2 回

反応条件

温度
40 °C

実験手順

To a solution of 362 g of sodium hydroxide in 362 ml of demineralized water 216.6 g of α-isopropyl-2-methylbenzyl cyanide and 6.4 g of tetrabutylammonium hydrogen sulfate were added, and the mixture was heated to 40° C. with intensive stirring. During 3hours 287 g of allylchloride was added. During, the addition and for further two hours the temperature of the reaction mixture was maintained at 40° C. and thereafter at 60° C. for additional three hours. After cooling to room temperature, the reaction mixture was diluted with 550 ml of water and the product was extracted into toluene. After washing with water until neutral pH and drying with anhydrous magnesium sulfate, the solvent was evaporated and the residue was distilled under diminished pressure to obtain 249 g (93%) of the desired compound, b.p. 122°-124 ° C./333 Pa.

後処理

  1. additionDuring, the addition
  2. temperaturefor further two hours the temperature of the reaction mixture was maintained at 40° C.
  3. temperatureAfter cooling to room temperature
  4. extractionthe product was extracted into toluene
  5. washAfter washing with water until neutral pH
  6. dry with materialdrying with anhydrous magnesium sulfate
  7. customthe solvent was evaporated
  8. distillationthe residue was distilled under diminished pressure

出典と根拠

ORDレコード
ord-4885e1af76354a0da3de3354ae290034
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05424456

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート