Potassium Carbonate → HCID 18780576、化合物

HRID 1421272

反応式

HRID 1421272 の反応式
[CH:1]1([NH2:11])[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[I-].C([N+]1(C)[CH2:26][CH2:25][C:24](=[O:27])[CH2:23][CH2:22]1)C.C([O-])(O)=O.[Na+]>C(O)C.O>[CH:1]1([N:11]2[CH2:26][CH2:25][C:24](=[O:27])[CH2:23][CH2:22]2)[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 573577CyclodecanamineHCID 110975681-Ethyl-1-methyl-4-oxopiperidin-1-ium iodide

生成物 1

HCID 18780576HCID 18780576、化合物収率 85%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of cyclodecylamine (6.78 g, 44 mmol) in ethanol (80 ml) was added a solution of potassium carbonate (0.60 g, 3.9 mmol) and 1-ethyl-1-methyl-4-oxo-piperidinium iodide (16.2 g, 60 mmol) in water (40 ml) and the mixture was refluxed for 100 min. The reaction mixture was poured into sat. NaHCO3 -solution (120 ml)/ice (400 ml) and extracted with ethylacetate (2×300 ml). The combined organic layers were dried (MgSO4) and evaporated. Column chromatography on silica gel (toluene/ethylacetate 2:1) yielded the title compound (8.8 g, 85%) as a pale brown oil, MS: m/e=238.4 (M+).

後処理

  1. temperaturethe mixture was refluxed for 100 min
  2. extractionextracted with ethylacetate (2×300 ml)
  3. dry with materialThe combined organic layers were dried (MgSO4)
  4. customevaporated

出典と根拠

ORDレコード
ord-39b93244ca404536900f5fff53df536d
出典データセット
uspto-grants-2000_06
特許番号
US06075034

関連ノート

読み込み中…