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

HRID 1195236ノート

反応式

HRID 1195236 の反応式
Cl.[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 19819017HCID 19819017、化合物

生成物 1

HCID 10878400Pyrrolizinium, 1,2,3,5,6,7-hexahydro-, perchlorate収率 400.4%

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 hydrochloride (1.00 g, 6.87 mmol) in 6.0 ml of dimethyl sulfoxide was added 1.68 g (1.37 mmol) of ammonium perchlorate. The mixture was heated with stirring at 100° C. for 6 hours. The solvent was distilled out in vacuo and isobutyl alcohol (6 ml) was added to the residue. Precipitated crystals was obtained and recrystallized from ethanol to afford 1.15 g (Yield: 80%) of the desired compound.

後処理

  1. temperatureThe mixture was heated
  2. distillationThe solvent was distilled out in vacuo and isobutyl alcohol (6 ml)
  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-e7af98f8f1474f33bb6573eff90da3f5
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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