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

HRID 2413332

반응식

HRID 2413332 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 12679Hexamethylphosphoramide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-16346bd1c6314838abc2eabb84ef2837
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04496720

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