Chloroacetonitrile → [(3,4-Dichlorophenyl)sulfanyl]acetonitrile

HRID 2413332

反応式

HRID 2413332 の反応式
Cl[CH2:2][C:3]#[N:4].[Cl:5][C:6]1[CH:7]=[C:8]([S:13][Si](C)(C)C)[CH:9]=[CH:10][C:11]=1[Cl:12]>C(#N)C.CN(C)P(=O)(N(C)C)N(C)C>[Cl:5][C:6]1[CH:7]=[C:8]([S:13][CH2:2][C:3]#[N:4])[CH:9]=[CH:10][C:11]=1[Cl:12]

参加物

5

反応物 2

HCID 7856ChloroacetonitrileHCID 20491069[(3,4-Dichlorophenyl)sulfanyl](trimethyl)silane

生成物 1

HCID 18542995[(3,4-Dichlorophenyl)sulfanyl]acetonitrile収率 96.9%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 12679Hexamethylphosphoramide溶媒

実験手順

3.5 ml (55 mmoles) of chloroacetonitrile were added to a refluxing solution of 11.0 g (44 mmoles) of 3,4-dichlorophenylthio(trimethyl)silane in a mixture of 25 ml of acetonitrile and 10 ml of hexamethylphosphoric triamide and the reaction was complete with 2 minutes. The residue obtained after evaporation of the acetonitrile was dissolved in ethyl acetate, and the solution was washed with water, dried and evaporated to dryness to obtain 9.30 g (93% yield) of (3,4-dichlorophenylthio)acetonitrile boiling at 127°-130° C./0.4 mm Hg and having a refractive index of nD25 =1.5920.

後処理

  1. customThe residue obtained
  2. customafter evaporation of the acetonitrile
  3. dissolutionwas dissolved in ethyl acetate
  4. washthe solution was washed with water
  5. customdried
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-16346bd1c6314838abc2eabb84ef2837
出典データセット
uspto-grants-1985_01
特許番号
US04496720

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