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Sodium Chloride → 2-Isopropyl-3-methylbutanenitrile

HRID 1680802
ノート
印刷プレビュー

反応式

HRID 1680802 の反応式
C(OC(=O)[C:5]([CH:11]([CH3:13])[CH3:12])([CH:8]([CH3:10])[CH3:9])[C:6]#[N:7])C.O=P1(C)CCC=C1.[Cl-].[Na+]>O>[CH:8]([CH:5]([CH:11]([CH3:13])[CH3:12])[C:6]#[N:7])([CH3:10])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5234Sodium ChlorideHCID 701042,3-Dihydro-1-methyl-1H-phosphole 1-oxideHCID 12463390Ethyl 2-cyano-3-methyl-2-(propan-2-yl)butanoate

生成物 1

HCID 136998412-Isopropyl-3-methylbutanenitrile収率 85%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

98.5 g (0.5 mol) of diisopropyl-cyanoacetic acid ethyl ester (prepared according to J. Chem. Soc., 1930, page 2,758), 300 ml of 1-oxo-1-methyl-phospholine, 31 g of sodium chloride and 22 g of water were heated to 160°-170° C. for 9 hours. After cooling, the mixture was diluted with 1,000 ml of water and extracted by shaking four times with 150 ml of petroleum ether each time. The combined petroleum ether phases were washed twice with 200 ml of water each time and dried with Na2SO4 and the petroleum ether was distilled off under normal pressure. The residual crude product was then purified by vacuum distillation. 53.2 g (85% of theory) of diisopropyl-acetonitrile of boiling point 60° C./14 mm Hg were obtained. Refractive index nD20 =1.4190.

後処理

  1. temperatureAfter cooling
  2. extractionextracted
  3. washThe combined petroleum ether phases were washed twice with 200 ml of water each time
  4. dry with materialdried with Na2SO4
  5. distillationthe petroleum ether was distilled off under normal pressure
  6. distillationThe residual crude product was then purified by vacuum distillation

出典と根拠

ORDレコード
ord-ee14cb9738184ddc95bd4954af833349
出典データセット
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04276225

反応ノート

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