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

HRID 1977

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

4

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
特許番号
US05728650

関連ノート

読み込み中…