Acetone → 2-Azidomethyl-2-hydroxy-1,3-diazidopropane

HRID 1760358

反応式

HRID 1760358 の反応式
[N:1]([CH2:4][C:5]([CH2:7][N:8]=[N+:9]=[N-:10])=[O:6])=[N+:2]=[N-:3].[N-:11]=[N+:12]=[N-:13].[Na+].[CH3:15]C(C)=O>>[N:1]([CH2:4][C:5]([OH:6])([CH2:15][N:11]=[N+:12]=[N-:13])[CH2:7][N:8]=[N+:9]=[N-:10])=[N+:2]=[N-:3]

参加物

4

反応物 3

HCID 180AcetoneHCID 33557Sodium AzideHCID 121381971,3-Diazidoacetone

生成物 1

HCID 121382042-Azidomethyl-2-hydroxy-1,3-diazidopropane

実験手順

To a solution of 1,3-diazidoacetone 7 (10 gms, 0.07 mol) in aq. acetone (20 mL water, 150 mL acetone) was added sodium azide (15 gm, 0.23 mol) and the resulting mixture was heated under reflux for 14 hours. The reaction mixture was concentrated under reduced pressure and partitioned between water and methylene chloride. The organic layer was separated, dried over sodium sulfate and concentrated to obtain a residue that was chromatographed to obtain pure 2-azidomethyl-2-hydroxy-1,3-diazidopropane 2.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 14 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. custompartitioned between water and methylene chloride
  5. customThe organic layer was separated
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated
  8. customto obtain a residue that
  9. customwas chromatographed

出典と根拠

ORDレコード
ord-6e474a4dc01046528f618561184b7614
出典データセット
uspto-grants-2005_01
特許番号
US06841690B1

関連ノート

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