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Dimethylformamide → HCID 68912756、化合物

HRID 732631
ノート
印刷プレビュー

反応式

HRID 732631 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:3][CH2:2]1.[C:12](=[O:15])([O-])[O-].[K+].[K+].BrCC(O[C:23]([CH3:26])([CH3:25])[CH3:24])=O.[CH3:27]N(C=O)C>C(OCC)C>[C:23]([C:12](=[O:15])[CH2:27][N:1]1[CH2:6][CH2:5][CH:4]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:3][CH2:2]1)([CH3:26])([CH3:25])[CH3:24]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 70770Ethyl 4-piperidinecarboxylateHCID 79177tert-Butyl bromoacetate

生成物 1

HCID 68912756HCID 68912756、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
60 °C

実験手順

A 5.00 g portion of ethyl piperidine-4-carboxylate was dissolved in 100 ml of DMF, and 6.52 g of potassium carbonate and 6.74 g of tert-butyl bromoacetate were added thereto and stirred at 60° C. for 5Hours. After spontaneous cooling, the reaction solution was diluted with diethyl ether, washed with water and saturated brine and dried with anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure, and the thus obtained residue was purified by a silica gel column chromatography (chloroform-methanol) to obtain 7.59 g of ethyl 1-(2-tert-butyl-2-oxoethyl)piperidine-4-carboxylate as a pale yellow oily substance.

後処理

  1. washwashed with water and saturated brine
  2. dry with materialdried with anhydrous sodium sulfate
  3. customThe solvent was evaporated under a reduced pressure
  4. customthe thus obtained residue was purified by a silica gel column chromatography (chloroform-methanol)

出典と根拠

ORDレコード
ord-74f77cbc96e44ae8a074644f2cd87db5
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07585886B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート