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

HRID 258120

반응식

HRID 258120 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 1364034191-Diethoxymethyl-2-nitroiminoimidazolidine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d6a20cb54b64732b2db00d40b533e37
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05264584

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