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Sodium Chloride → 2-Isopropyl-3-methylbutanenitrile

HRID 1680802
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반응식

HRID 1680802 반응식
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]
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참가 물질

5

반응물 3

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

생성물 1

HCID 136998412-Isopropyl-3-methylbutanenitrile수율 85%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ee14cb9738184ddc95bd4954af833349
출처 데이터셋
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04276225

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