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2-Amino-2,4-dimethylpentanenitrile → 2,2'-Azobis(2,4-dimethylvaleronitrile)

HRID 1680123
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HRID 1680123 반응식
Cl[O-].[Na+].[NH2:4][C:5]([CH3:12])([CH2:8][CH:9]([CH3:11])[CH3:10])[C:6]#[N:7]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C(OCC)(=O)C>[N:4]([C:5]([CH3:12])([CH2:8][CH:9]([CH3:11])[CH3:10])[C:6]#[N:7])=[N:4][C:5]([CH3:12])([CH2:8][CH:9]([CH3:11])[CH3:10])[C:6]#[N:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 922512-Amino-2,4-dimethylpentanenitrileHCID 23665760Sodium Hypochlorite

생성물 1

HCID 915372,2'-Azobis(2,4-dimethylvaleronitrile)

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 8857Ethyl Acetate용매

실험 절차

Next, 213 g of a 10% aqueous sodium hypochlorite solution was cooled to 5° C. and 0.5 g of benzyltriethylammonium chloride was added thereto. To the resulting aqueous solution was added 200 ml of an ethyl acetate solution containing 33 g of the resulting 90%-pure 2-amino-2,4-dimethylpentanonitrile over 30 minutes with stirring. This reaction mixture was stirred at 5° to 10° C. for 3 hours, and the organic and water phases were separated from each other. Ethyl acetate was removed from the organic phase under reduced pressure. The resulting white crystals were washed with water and dried to obtain 24.8 g of 2,2'-azobis(2,4-dimethylpentanonitrile). Yield was 85 mole %.

후처리

  1. stirringThis reaction mixture was stirred at 5° to 10° C. for 3 hours
  2. customthe organic and water phases were separated from each other
  3. customEthyl acetate was removed from the organic phase under reduced pressure
  4. washThe resulting white crystals were washed with water
  5. customdried

출처 및 근거

ORD 기록
ord-576ef44274384349824c609c27eacc47
출처 데이터셋
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04272435

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