ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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

HRID 2021
ノート
印刷プレビュー

反応式

HRID 2021 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8959e916559b4ac888f77a67d88387d1
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05728686

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート