Hydrochloric Acid → 1-Ethylcarbonyl-4-oxohomopiperidine

HRID 917062ノート

反応式

HRID 917062 の反応式
[O:1]=[C:2]1[CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.Cl.[C:10]([O-:13])([O-])=O.[K+].[K+].ClC(O[CH2:20][CH3:21])=O>C1COCC1>[CH2:20]([C:10]([N:5]1[CH2:6][CH2:7][CH2:8][C:2](=[O:1])[CH2:3][CH2:4]1)=[O:13])[CH3:21]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 1501891Azepan-4-one

生成物 1

HCID 186757361-Ethylcarbonyl-4-oxohomopiperidine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a cold (0° C.) stirred solution of 4-oxohomopiperidine.HCl (0.6 g, 4.05 mmol), K2CO3 (0.615 g, 4.46 mmol) in anhydrous THF (10 mL) will be ethyl chloroformate (0.44 mL, 4.05 mmol) dropwise. The reaction was warmed to RT for 2 hrs then quenched with H2O, extracted with EtOAc, and the organic layer dried over Na2SO4. Pure 1-ethylcarbonyl-4-oxohomopiperidine will be isolated via silica gel flash chromatography.

後処理

  1. customthen quenched with H2O
  2. extractionextracted with EtOAc
  3. dry with materialthe organic layer dried over Na2SO4

出典と根拠

ORDレコード
ord-b80128a1be7e48e6b0fd10cc8840b5a2
出典データセット
uspto-grants-2007_09
特許番号
US07271176B2

反応ノート

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