Carbon Dioxide → 3,3-Dinitroazetidinium trifluoromethanesulfonate

HRID 1608674노트

반응식

HRID 1608674 반응식
C(OC([N:11]1[CH2:14][C:13]([N+:18]([O-:20])=[O:19])([N+:15]([O-:17])=[O:16])[CH2:12]1)=O)C1C=CC=CC=1.C1(OC)C=CC=CC=1.[F:29][C:30]([F:36])([F:35])[S:31]([OH:34])(=[O:33])=[O:32].C(=O)=O>C(Cl)Cl.C(OCC)C>[F:29][C:30]([F:36])([F:35])[S:31]([O-:34])(=[O:33])=[O:32].[N+:15]([C:13]1([N+:18]([O-:20])=[O:19])[CH2:14][NH2+:11][CH2:12]1)([O-:17])=[O:16]

참가 물질

7

반응물 4

HCID 280Carbon DioxideHCID 7519AnisoleHCID 62406Trifluoromethanesulfonic acidHCID 104464271-Azetidinecarboxylic acid, 3,3-dinitro-, phenylmethyl ester

생성물 1

HCID 200870453,3-Dinitroazetidinium trifluoromethanesulfonate수율 97%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(benzyloxycarbonyl)-3,3-dinitroazetidine (8.0 g, 0.028 mole) in 80 ml of methylene chloride containing anisole (9.24 g, 0.08 mole) was added trifluoromethanesulfonic acid (10 g, 0.067 mole), slowly with vigorous stirring at room temperature. Carbon dioxide was evolved and the solution turned light red in color. Stirring was continued for about 30 minutes after the addition. Diethyl ether was added slowly to quench the reaction and precipitate the resultant product. The solids were filtered, washed with diethyl ether and air-dried to give 4.10 g (97% yield) of pure 3,3-dinitroazetidinium trifluoromethanesulfonate. The melting point of the product was 176° (dec.).

후처리

  1. stirringStirring
  2. additionafter the addition
  3. customto quench
  4. customthe reaction
  5. customprecipitate the resultant product
  6. filtrationThe solids were filtered
  7. washwashed with diethyl ether
  8. customair-dried

출처 및 근거

ORD 기록
ord-59a8979f1dfa4deeb83f8064dc94f4c6
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05395945

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