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

HRID 1195237ノート

反応式

HRID 1195237 の反応式
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

参加物

4

反応物 2

HCID 24639Ammonium perchlorateHCID 19819013HCID 19819013、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-96ec4aa98ca345209bdca8f0a32053a8
出典データセット
uspto-grants-1992_05
特許番号
US05110945

反応ノート

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