Dimethyl Sulfoxide → HCID 54378726、化合物

HRID 1033543ノート

反応式

HRID 1033543 の反応式
[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

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 1554792-Chloro-5-(chloromethyl)pyridineHCID 136378393HCID 136378393、化合物

生成物 1

HCID 54378726HCID 54378726、化合物収率 71.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8d2e71d3fbde4ad5b50873edfa238471
出典データセット
uspto-grants-1994_05
特許番号
US05310920

反応ノート

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