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Bromotrimethylsilane → 3-Aminooctane-1,1-bisphosphonic acid, triammonium salt

HRID 1977
ノート
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反応式

HRID 1977 の反応式
[NH2:1][CH:2]([CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:3][CH:4]([P:13]([O:18]CC)(=[O:17])[O:14]CC)[P:5]([O:10]CC)(=[O:9])[O:6]CC.Br[Si](C)(C)C>ClCCl>[NH4+:1].[NH4+:1].[NH4+:1].[NH2:1][CH:2]([CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:3][CH:4]([P:5]([O-:10])(=[O:6])[OH:9])[P:13]([O-:18])(=[O:14])[O-:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 76113BromotrimethylsilaneHCID 19689051Tetraethyl 3-aminooctane-1,1-bisphosphonate

生成物 1

HCID 1317205653-Aminooctane-1,1-bisphosphonic acid, triammonium salt収率 419.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tetraethyl 3-aminooctane-1,1-bisphosphonate (0.45 g, 1.12 mmol) in dry dichloromethane (1.1 mL) was added bromotrimethylsilane (1.05 mL, 7.85 mmol) via syringe. After 18 hours, the mixture was concentrated under vacuum. To the residue was added 3N NH4OH (8 mL) which was stirred for 30 minutes at room temperature. The solvent was removed in vacuo and the residue concentrated from methanol (2 mL) to give 0.40 g of 3-aminooctane-1,1-bisphosphonic acid, triammonium salt as a white powder.

後処理

  1. concentrationthe mixture was concentrated under vacuum
  2. additionTo the residue was added 3N NH4OH (8 mL) which
  3. customThe solvent was removed in vacuo
  4. concentrationthe residue concentrated from methanol (2 mL)

出典と根拠

ORDレコード
ord-66715e3038e443c89124069570855fa8
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05728650

反応ノート

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