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

HRID 353420ノート

反応式

HRID 353420 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-a3b9080ec2d24822b33cf252aa890ae6
出典データセット
uspto-grants-2004_06
特許番号
US06753324B2

反応ノート

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