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Ammonia → Diammonium [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate

HRID 2021
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HRID 2021 반응식
C[Si](Br)(C)C.[CH2:6]([O:8][CH2:9][N:10]1[C:18]2[C:17](=[O:19])[N:16]([CH2:20][CH2:21][CH2:22][CH2:23][P:24](=[O:27])([O-:26])[O-:25])[C:15](=[O:28])[N:14]([CH3:29])[C:13]=2[N:12]=[CH:11]1)[CH3:7].CO.[NH3:32]>ClCCl>[CH2:6]([O:8][CH2:9][N:10]1[C:18]2[C:17](=[O:19])[N:16]([CH2:20][CH2:21][CH2:22][CH2:23][P:24](=[O:25])([O-:27])[O-:26])[C:15](=[O:28])[N:14]([CH3:29])[C:13]=2[N:12]=[CH:11]1)[CH3:7].[NH4+:32].[NH4+:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 887MethanolHCID 76113BromotrimethylsilaneHCID 19689210[4-(7-Ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate

생성물 1

HCID 86752277Diammonium [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

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온도
0 °C

실험 절차

3.4 ml (0.026 mol) of trimethylsilyl bromide were slowly added dropwise at 0° C., under an argon atmosphere, to a solution of 4.16 g (0.01 mol) of [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate in 5 ml of dichloromethane. The solution was stirred at 0° C. for 1 hour and at room temperature for 2 hours. The dichloromethane was then evaporated and the oily residue which remained was dried in a bulb tube in an oil pump vacuum to remove excess trimethylsilyl bromide and ethyl bromide formed. The residue was taken up in a little methanol and treated with 1 ml of concentrated ammonia solution and stirred at room temperature for 2 hours. After evaporating the solvent, the diammonium salt was crystallized from a methanoltdiisopropyl ether mixture.

후처리

  1. customThe dichloromethane was then evaporated
  2. customthe oily residue which remained was dried in a bulb tube in an oil pump vacuum
  3. customto remove excess trimethylsilyl bromide and ethyl bromide
  4. customformed
  5. stirringstirred at room temperature for 2 hours
  6. customAfter evaporating the solvent
  7. customthe diammonium salt was crystallized from a methanoltdiisopropyl ether mixture

출처 및 근거

ORD 기록
ord-8959e916559b4ac888f77a67d88387d1
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05728686

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