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

HRID 1885601ノート

反応式

HRID 1885601 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 198793522-(3,4-Dichlorophenylthiomethyl)glutaronitrile

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6cc0bbfeb3ad4443b7da709c89e08b7d
出典データセット
uspto-grants-1992_09
特許番号
US05145869

反応ノート

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