Sodium Azide → (2-Azido-ethoxy)methyl-phosphonic acid-diethylester

HRID 2414236ノート

反応式

HRID 2414236 の反応式
[CH2:1]([O:3][P:4]([CH2:9][O:10][CH2:11][CH2:12]Cl)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[N-:14]=[N+:15]=[N-:16].[Na+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH2:1]([O:3][P:4]([CH2:9][O:10][CH2:11][CH2:12][N:14]=[N+:15]=[N-:16])(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2]

参加物

5

反応物 2

HCID 33557Sodium AzideHCID 10014096Diethyl ((2-chloroethoxy)methyl)phosphonate

生成物 1

HCID 10037145(2-Azido-ethoxy)methyl-phosphonic acid-diethylester

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 1140Toluene溶媒

実験手順

0,02 mol (2-chloroethoxy)methyl-phosphonic acid diethylester, 3 mmol tetrabutylammoniumbromide and 2,5 g sodiumazide are boiled in 50 ml toluol under reflux for 4 h. After cooling-off it is washed for three times with 25 ml water respectively. The watery phase may be extracted with toluol. The combined toluol phases are dried over sodiumsulfate and the solvent is removed in the vacuum. A yellow oil remains.

後処理

  1. temperatureunder reflux for 4 h
  2. washAfter cooling-off it is washed for three times with 25 ml water respectively
  3. extractionThe watery phase may be extracted with toluol
  4. dry with materialThe combined toluol phases are dried over sodiumsulfate
  5. customthe solvent is removed in the vacuum

出典と根拠

ORDレコード
ord-1cc503066660426d933cb30d1cdcce9e
出典データセット
uspto-grants-2004_11
特許番号
US06812224B2

反応ノート

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