Dimethyl Sulfoxide → HCID 54378726, 화합물

HRID 1033543노트

반응식

HRID 1033543 반응식
[O:1]([CH:8]=[CH:9][N:10]1[CH2:14][CH2:13][NH:12][C:11]1=[N:15][N+:16]([O-:18])=[O:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26]Cl)=[CH:22][N:21]=1.C(=O)([O-])[O-].[K+].[K+].CS(C)=O>O>[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][N:12]2[CH2:13][CH2:14][N:10]([CH:9]=[CH:8][O:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:11]2=[N:15][N+:16]([O-:18])=[O:17])=[CH:22][N:21]=1

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 1554792-Chloro-5-(chloromethyl)pyridineHCID 136378393HCID 136378393, 화합물

생성물 1

HCID 54378726HCID 54378726, 화합물수율 71.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

A mixture comprising 2.8 g of 1-(2-phenoxyvinyl)2-nitroiminoimidazolidine, 3.6 g of 2-chloro-5chloromethylpyridine, 3.2 g of potassium carbonate and 15 ml of dimethylsulfoxide was stirred at 70° C. for one hour. The reaction mixture was poured into water, extracted with ethyl acetate, washed with water, dried (with anhydrous MgSO4) and concentrated to give an oily residue. This was purified by column chromatography (silica gel, eluet: ethyl acetate) to give 3.0 g of 1-(2-chloropyridin-5-ylmethyl)-2-nitroimino-3-(2-phenoxyvinyl)-imidazolidine.

후처리

  1. extractionextracted with ethyl acetate
  2. washwashed with water
  3. dry with materialdried (with anhydrous MgSO4)
  4. concentrationconcentrated
  5. customto give an oily residue
  6. customThis was purified by column chromatography (silica gel, eluet: ethyl acetate)

출처 및 근거

ORD 기록
ord-8d2e71d3fbde4ad5b50873edfa238471
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310920

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