Ammonium perchlorate → Pyrrolizinium, 1,2,3,5,6,7-hexahydro-, perchlorate

HRID 1195237노트

반응식

HRID 1195237 반응식
Br.[CH:2]1([C:5]([CH:7]2[CH2:9][CH2:8]2)=[NH:6])[CH2:4][CH2:3]1.[Cl:10]([O-:14])(=[O:13])(=[O:12])=[O:11].[NH4+]>CS(C)=O>[Cl:10]([O-:14])(=[O:13])(=[O:12])=[O:11].[N+:6]12[CH2:9][CH2:8][CH2:7][C:5]=1[CH2:2][CH2:3][CH2:4]2

참가 물질

4

반응물 2

HCID 24639Ammonium perchlorateHCID 19819013HCID 19819013, 화합물

생성물 1

HCID 10878400Pyrrolizinium, 1,2,3,5,6,7-hexahydro-, perchlorate수율 82%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
100 °C

실험 절차

To a solution of dicyclopropylmethanimine hydrobromide (1.00 g, 5.26 mmol) in 6.0 ml of dimethyl sulfoxide was added 1.29 g (10.5 mmol) of ammonium perchlorate. The mixture was heated with stirring at 100° C. for 1 hour. The solvent was distilled out in vacuo and isobutyl alcohol was added to the residue. Precipitated crystals was obtained and recrystallized from ethanol to afford 0.90 g (Yield: 82%) of the desired compound.

후처리

  1. temperatureThe mixture was heated
  2. distillationThe solvent was distilled out in vacuo and isobutyl alcohol
  3. additionwas added to the residue
  4. customPrecipitated crystals
  5. customwas obtained
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-96ec4aa98ca345209bdca8f0a32053a8
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05110945

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