Ethanol → 2-(3,4-Dichlorophenylthiomethyl)glutaronitrile

HRID 1885601노트

반응식

HRID 1885601 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([SH:9])[CH:5]=[CH:6][C:7]=1[Cl:8].[CH2:10]=[C:11]([CH2:14][CH2:15][C:16]#[N:17])[C:12]#[N:13].C(O)C>CO>[Cl:1][C:2]1[CH:3]=[C:4]([S:9][CH2:10][CH:11]([CH2:14][CH2:15][C:16]#[N:17])[C:12]#[N:13])[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

5

반응물 3

HCID 702EthanolHCID 740802,4-Dicyano-1-buteneHCID 799643,4-Dichlorobenzenethiol

생성물 1

HCID 198793522-(3,4-Dichlorophenylthiomethyl)glutaronitrile

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 3,4-dichlorobenzenethiol (3.00 ml), methyleneglutaronitrile (2.57 ml), ethanol (25 ml), and triton B (40% methanol solution, 10 drops) was refluxed for 4 hours. After the reaction mixture was concentrated in vacuo, the resulting residue was dissolved in chloroform, washed with water, and dried over MgSO4. The solvent was evaporated at reduced pressure, and the residue was recrystallized from diethyl ether-hexane to give 6.14 g of 2-(3,4-dichlorophenylthiomethyl)glutaronitrile.

후처리

  1. temperaturewas refluxed for 4 hours
  2. concentrationAfter the reaction mixture was concentrated in vacuo
  3. dissolutionthe resulting residue was dissolved in chloroform
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. customThe solvent was evaporated at reduced pressure
  7. customthe residue was recrystallized from diethyl ether-hexane

출처 및 근거

ORD 기록
ord-6cc0bbfeb3ad4443b7da709c89e08b7d
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05145869

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