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2,6-Dimethylaniline → (2,6-Dimethylanilino)acetonitrile

HRID 2285942
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HRID 2285942 반응식
C1(S([O-])(=O)=O)C=CC=CC=1.[C:11](#[N:13])[CH3:12].[CH3:14][C:15]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[C:16]=1[NH2:17]>C(OCC)(=O)C>[CH3:14][C:15]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[C:16]=1[NH:17][CH2:12][C:11]#[N:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 68962,6-DimethylanilineHCID 86738343HCID 86738343, 화합물

생성물 1

HCID 20478053(2,6-Dimethylanilino)acetonitrile

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 158.5 g (0.804 mol) of benzenesulphonate-acetonitrile in 200 ml of ethyl acetate is run dropwise into a solution of 193.6 g (1.608 mols) of 2,6-dimethyl-aniline in 400 ml of ethyl acetate. The mixture is heated under reflux for 3 hours, cooled and the excess aniline benzenesulphonate is filtered off. The filtrate is evaporated to dryness. The residue is taken up in ether. Insoluble material is again filtered off and discarded. The ether is evaporated to dryness. The residue is taken up in a mixture of petroleum ether/benzene (3:4 v/v). The crystals which form are filtered off.

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후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 3 hours
  3. temperaturecooled
  4. filtrationthe excess aniline benzenesulphonate is filtered off
  5. customThe filtrate is evaporated to dryness
  6. filtrationInsoluble material is again filtered off
  7. customThe ether is evaporated to dryness
  8. additionThe residue is taken up in a mixture of petroleum ether/benzene (3:4 v/v)
  9. filtrationThe crystals which form are filtered off

출처 및 근거

ORD 기록
ord-80aecad225ff4701acbe0d42ff2af916
출처 데이터셋
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04325964

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