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Dimethylformamide → Cyclonon-1-ene-1-carbaldehyde

HRID 1169394
ノート
印刷プレビュー

反応式

HRID 1169394 の反応式
C1(C)C=CC(S(NN=[C:12]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)(=O)=O)=CC=1.C([Li])CCC.CN([CH:30]=[O:31])C>CCN(CCN(CC)CC)CC.CCCCCC>[C:12]1([CH:30]=[O:31])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH:20]=1
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 3

HCID 6228DimethylformamideHCID 85849656Cyclononanone p-toluenesulfonyl hydrazoneHCID 178418339Butyllithium

生成物 1

HCID 53877429Cyclonon-1-ene-1-carbaldehyde

試薬・触媒・溶媒 2

HCID 8058Hexane溶媒HCID 674231,2-Ethanediamine, N1,N1,N2,N2-tetraethyl-溶媒

実験手順

To cyclononanone p-toluenesulfonyl hydrazone (2.0 g) suspended in N,N,N′,N′-tetraethylenediamine (20 ml) was added dropwise at −55° C. a 1.6 M solution of n-butyllithium in hexane (16.2 ml). The resulting mixture was stirred at room temperature for 30 minutes under an argon atmosphere, was then cooled with ice, was mixed with DMF (2.5 ml) and was stirred at room temperature for one hour. The reaction mixture was poured into ice water and was extracted with ethyl acetate. The organic layer was washed with 1 N hydrochloric acid, water and an aqueous saturated solution of sodium chloride, and was then dried with anhydrous magnesium sulfate. The resulting organic layer was evaporated under reduced pressure to remove the solvent. The residue was subjected to purification using a silica gel column (ethyl acetate:hexane=1:10) to obtain cyclononene-1-carbaldehyde (0.7 g) as a light yellow oil.

後処理

  1. temperaturewas then cooled with ice
  2. stirringwas stirred at room temperature for one hour
  3. extractionwas extracted with ethyl acetate
  4. washThe organic layer was washed with 1 N hydrochloric acid, water
  5. dry with materialan aqueous saturated solution of sodium chloride, and was then dried with anhydrous magnesium sulfate
  6. customThe resulting organic layer was evaporated under reduced pressure
  7. customto remove the solvent
  8. customThe residue was subjected to purification

出典と根拠

ORDレコード
ord-8d25e1a21d8d48c68c5b247e5bbfafed
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06627651B1

反応ノート

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