1,3-Dimethyl-2-imidazolidinone → 1-Diethoxymethyl-2-nitroiminoimidazolidine

HRID 258120

反応式

HRID 258120 の反応式
[N+:1]([N:4]=[C:5]1[NH:9][CH2:8][CH2:7][NH:6]1)([O-:3])=[O:2].[CH:10]([O-:15])([O-])[O:11][CH2:12][CH3:13].CN1[CH2:21][CH2:20]N(C)C1=O>O>[CH2:20]([O:15][CH:10]([O:11][CH2:12][CH3:13])[N:6]1[CH2:7][CH2:8][NH:9][C:5]1=[N:4][N+:1]([O-:3])=[O:2])[CH3:21]

参加物

5

反応物 3

HCID 66611,3-Dimethyl-2-imidazolidinoneHCID 53630039EthylorthoformateHCID 135413413N-nitroimidazolidin-2-imine

生成物 1

HCID 1364034191-Diethoxymethyl-2-nitroiminoimidazolidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 25 g of 2-nitroiminoimidazolidine, 100 g of ethyl orthoformate and 25 ml of 1,3-dimethyl-2-imidazolidinone was heated under reflux for 3 hours. After cooling to room temperature, the mixture was poured into water, followed by extraction with ethyl acetate. After washing with water, the extract was dried with anhydrous magnesium sulfate, after which the solvent was distilled off under reduced pressure. The resultant crystals were sludged with ether to give 32 g of 1-diethoxymethyl-2-nitroiminoimidazolidine.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. extractionfollowed by extraction with ethyl acetate
  4. washAfter washing with water
  5. dry with materialthe extract was dried with anhydrous magnesium sulfate
  6. distillationafter which the solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-6d6a20cb54b64732b2db00d40b533e37
出典データセット
uspto-grants-1993_11
特許番号
US05264584

関連ノート

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