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Water → HCID 22243702、化合物

HRID 890923
ノート
印刷プレビュー

反応式

HRID 890923 の反応式
[CH3:1][O:2][C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][CH2:10][C:11]([OH:13])=O)=[O:8])=[CH:5][CH:4]=1.C1(N=C=NC2CCCCC2)CCCCC1.[N:31]12[CH2:39][CH2:38][CH:35]([CH2:36][CH2:37]1)[NH:34][CH2:33][CH2:32]2.O>O1CCOCC1>[N:31]12[CH2:39][CH2:38][CH:35]([CH2:36][CH2:37]1)[N:34]([C:11](=[O:13])[CH2:10][NH:9][C:7](=[O:8])[C:6]1[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:15][CH:14]=1)[CH2:33][CH2:32]2
参加物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 962WaterHCID 10868DicyclohexylcarbodiimideHCID 1288474-Methyoxybenzoyl-N-glycineHCID 3984071,4-Diazabicyclo(3.2.2)nonane

生成物 1

HCID 22243702HCID 22243702、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.42 g (2 mmol) of N-(4-methoxybenzoyl)glycine dissolved in 20 ml of dioxane is placed in a 50 ml round-bottomed flask, 0.45 g (2.2 mmol) of dicyclohexylcarbodiimide is added, the mixture is stirred at room temperature for 30 minutes, 0.25 g (2 mmol) of 1,4-diazabicyclo[3.2.2]nonane is added and the mixture is stirred for a further one hour. 20 ml of water are added, the precipitate formed is filtered off, the filtrate is extracted with chloroform, the organic phase is extracted with aqueous 0.1N hydrochloric acid solution and the aqueous extraction phase is basified to pH 10 by addition of concentrated aqueous sodium hydroxide solution and extracted with chloroform. The organic phase is dried over sodium sulfate and concentrated under reduced pressure.

後処理

  1. customis placed in a 50 ml round-bottomed flask
  2. stirringthe mixture is stirred for a further one hour
  3. customthe precipitate formed
  4. filtrationis filtered off
  5. extractionthe filtrate is extracted with chloroform
  6. extractionthe organic phase is extracted with aqueous 0.1N hydrochloric acid solution
  7. additionthe aqueous extraction phase is basified to pH 10 by addition of concentrated aqueous sodium hydroxide solution
  8. extractionextracted with chloroform
  9. dry with materialThe organic phase is dried over sodium sulfate
  10. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-beea767faf5d462a9846784031cefb0a
出典データセット
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07001902B2

反応ノート

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