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

HRID 1977

반응식

HRID 1977 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 1317205653-Aminooctane-1,1-bisphosphonic acid, triammonium salt수율 419.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-66715e3038e443c89124069570855fa8
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728650

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