Sodium Iodide → 2-[2-Methoxy-3-(2-chlorophenylthio)phenyl]acetonitrile

HRID 1164081노트

반응식

HRID 1164081 반응식
[CH3:1][O:2][C:3]1[C:8]([CH2:9]Cl)=[CH:7][CH:6]=[CH:5][C:4]=1[S:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:18].[I-].[Na+].[C-:21]#[N:22].[K+]>CS(C)=O>[CH3:1][O:2][C:3]1[C:4]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])=[CH:5][CH:6]=[CH:7][C:8]=1[CH2:9][C:21]#[N:22]

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 9032Potassium CyanideHCID 205134642-Chlorophenyl 2-methoxy-3-chloromethylphenyl thioether

생성물 1

HCID 205134652-[2-Methoxy-3-(2-chlorophenylthio)phenyl]acetonitrile수율 99.9%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 2-chlorophenyl 2-methoxy-3-chloromethylphenyl thioether (9.2 g) and sodium iodide (4.8 g) in dimethyl sulfoxide (50 ml) was stirred at room temperature. To the mixture was added powdered potassium cyanide (2.1 g) all at once, and the mixture was stirred at 70° C. for 3 hours. The reaction mixture was poured into ice-water and extracted with diethyl ether. The extract was washed with water, dried and then evaporated to give oily 2-[2-methoxy-3-(2-chlorophenylthio)phenyl]acetonitrile (8.9 g). This product was purified by column chromatography (silica gel 150 g, benzene) to give purified oily product (4.1 g).

후처리

  1. stirringwas stirred at 70° C. for 3 hours
  2. extractionextracted with diethyl ether
  3. washThe extract was washed with water
  4. customdried
  5. customevaporated

출처 및 근거

ORD 기록
ord-ebd4cf41353b463da36c5bcd7b307108
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04367238

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