Pyridine → 1-[2-Chloro-4-(3-chlorophenoxy)phenoxy]-2-[N-ethyl-N-(4-chlorophenylsulfenyl)aminocarbonyloxy]ethane

HRID 265624노트

반응식

HRID 265624 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]Cl)=[CH:4][CH:3]=1.C1(C)C=CC=CC=1.[Cl:17][C:18]1[CH:32]=[C:31]([O:33][C:34]2[CH:39]=[CH:38][CH:37]=[C:36]([Cl:40])[CH:35]=2)[CH:30]=[CH:29][C:19]=1[O:20][CH2:21][CH2:22][O:23][C:24]([NH:26][CH2:27][CH3:28])=[O:25].N1C=CC=CC=1>CCOCC>[Cl:17][C:18]1[CH:32]=[C:31]([O:33][C:34]2[CH:39]=[CH:38][CH:37]=[C:36]([Cl:40])[CH:35]=2)[CH:30]=[CH:29][C:19]=1[O:20][CH2:21][CH2:22][O:23][C:24]([N:26]([CH2:27][CH3:28])[S:8][C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1)=[O:25]

참가 물질

6

반응물 4

HCID 1049PyridineHCID 1140Toluene2회HCID 110844654-ChlorobenzenesulfenylchlorideHCID 20088570HCID 20088570, 화합물

생성물 1

HCID 190345771-[2-Chloro-4-(3-chlorophenoxy)phenoxy]-2-[N-ethyl-N-(4-chlorophenylsulfenyl)aminocarbonyloxy]ethane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of 2 g of 4-chlorophenylsulfenyl chloride in 1 0 ml of toluene is added dropwise with stirring at 0°-5° C. in the course of approximately 30 minutes to a mixture of 3.7 g of 1-[2-chloro-4-(3-chlorophenoxy)phenoxy]2-ethylaminocarbonyloxyethane, 10 ml of pyridine and 10 ml of toluene, and stirring is continued for 16 hours at room temperature. The reaction mixture is diluted with 100 ml of ether, washed three times using ice-cold 1N hydrochloric acid and three times using water, the organic phase is dried over sodium sulfate and the solvent is evaporated in vacuo. The crude product is purified on silica gel using diethyl ether/n-hexane (1:3) as mobile phase. This gives the title compound of refractive index nD20 1.6209.

후처리

  1. washwashed three times
  2. dry with materialthe organic phase is dried over sodium sulfate
  3. customthe solvent is evaporated in vacuo
  4. customThe crude product is purified on silica gel

출처 및 근거

ORD 기록
ord-f3ec063891e54068a8275cf34cb46b2c
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648494

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