Potassium Carbonate → HCID 178451986、化合物

HRID 1408339ノート

反応式

HRID 1408339 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]#[N:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])([O-])=O.[K+].[K+].Cl.[NH2:23][OH:24]>O.CCO>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[NH:15])[NH:23][OH:24])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 1514443Tert-butyl 4-cyanopiperidine-1-carboxylate

生成物 1

HCID 178451986HCID 178451986、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a mixture of 4-cyano-piperidine-1-carboxylic acid tert-butyl ester (6.3 g, 30 mmol), K2CO3 (4.2 g, 30 mmol) in H2O (50 mL) and EtOH (30 mL) was added hydroxylamine hydrogenchloride (4.17 g, 60 mmol). The mixture was heated under reflux overnight, cooled to room temperature and ethanol was removed in vacuo. The residue was extracted with EtOAc (300 mL). The organic layer was washed successively with H2O and brine. After drying (Na2SO4), the solvent was removed to afford the desired product.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux overnight
  3. customethanol was removed in vacuo
  4. extractionThe residue was extracted with EtOAc (300 mL)
  5. washThe organic layer was washed successively with H2O and brine
  6. dry with materialAfter drying (Na2SO4)
  7. customthe solvent was removed

出典と根拠

ORDレコード
ord-e536042bad33491cb5cec88fb0db431a
出典データセット
uspto-grants-2014_12
特許番号
US08921350B2

反応ノート

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