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

HRID 353420노트

반응식

HRID 353420 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a3b9080ec2d24822b33cf252aa890ae6
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06753324B2

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