Hydrochloric Acid → 1-Ethylcarbonyl-4-oxohomopiperidine

HRID 457047ノート

反応式

HRID 457047 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-651e4369b41c4937b002b3e1aa26a4e2
出典データセット
uspto-grants-2007_03
特許番号
US07186729B2

反応ノート

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