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Dimethyl Sulfoxide → HCID 53922531、化合物

HRID 1613216
ノート
印刷プレビュー

反応式

HRID 1613216 の反応式
[Cl:1][CH2:2][CH2:3][O:4][CH:5]([O:15][CH2:16][CH2:17][Cl:18])[N:6]1[CH2:10][CH2:9][NH:8][C:7]1=[N:11][N+:12]([O-:14])=[O:13].C(=O)([O-])[O-].[K+].[K+].[Cl:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32]Cl)=[CH:28][N:27]=1.CS(C)=O>O>[Cl:1][CH2:2][CH2:3][O:4][CH:5]([O:15][CH2:16][CH2:17][Cl:18])[N:6]1[CH2:10][CH2:9][N:8]([CH2:32][C:29]2[CH:30]=[CH:31][C:26]([Cl:25])=[N:27][CH:28]=2)[C:7]1=[N:11][N+:12]([O-:14])=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 1554792-Chloro-5-(chloromethyl)pyridineHCID 136403418HCID 136403418、化合物

生成物 1

HCID 53922531HCID 53922531、化合物収率 61.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

16.0 g of 1-[bis-(2-chloroethoxy)methyl]-2-nitroiminoimidazolidine, 13.0 g of anhydrous potassium carbonate, 13.0 g of 2-chloro-5-chloromethylpyridine and 70 ml of dimethyl sulfoxide were agitated at 70° C. for 1 hour. The reaction mixture was poured into water, and extracted with ethyl acetate. After washing with water, the extract was dried with anhydrous sodium sulfate, after which the solvent was distilled off under reduced pressure. The resultant oily residue was purified by column chromatography [silica gel, eluant: hexane/ethyl acetate (1:2)] to give 14.0 g of 1-[bis-(2-chloroethoxy)-methyl]-2-nitroimino-3-(2-chloropyridin-5-ylmethyl)imidazolidine.

後処理

  1. extractionextracted with ethyl acetate
  2. washAfter washing with water
  3. dry with materialthe extract was dried with anhydrous sodium sulfate
  4. distillationafter which the solvent was distilled off under reduced pressure
  5. customThe resultant oily residue was purified by column chromatography [silica gel, eluant: hexane/ethyl acetate (1:2)]

出典と根拠

ORDレコード
ord-fc77a698237642f68736baad7b99d855
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05192778

反応ノート

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