Bromotrimethylsilane → HCID 19756885, compound

HRID 1588056Notes

Reaction equation

HRID 1588056 reaction equation
C([O:3][P:4]([C:9]1([P:18](=[O:25])([O:22]CC)[O:19]CC)[CH2:13][C:12]([C:14](=[O:17])[CH2:15][CH3:16])=[N:11][NH:10]1)(=[O:8])[O:5]CC)C.Br[Si](C)(C)C>C(Cl)(Cl)Cl>[O:17]=[C:14]([C:12]1[CH2:13][C:9]([P:18](=[O:19])([OH:25])[OH:22])([P:4](=[O:3])([OH:8])[OH:5])[NH:10][N:11]=1)[CH2:15][CH3:16]

Participants

4

Reactant 2

HCID 76113BromotrimethylsilaneHCID 10000902HCID 10000902, compound

Product 1

HCID 19756885HCID 19756885, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

[2,4-Dihydro-5-(1-oxopropyl)-3H-pyrazol-3-ylidene]bisphosphonic acid tetraethyl ester (III, EXAMPLE 12, 1.56 g) and bromotrimethylsilane (2.6 ml) in chloroform (20 ml) are stirred at 50° for 4 hrs, then concentrated. The concentrate is diluted with water and ethyl acetate, shaken, and the aqueous layer separated and freeze dried to give the title compound, mp 148° foamed, IR (mineral oil mull) 3325, 1597, 1532, 1430, 1189, 1173, 1060, 1019 and 937 cm-1 ; NMR (D2O) 3.40, 2.84 and 1.07 δ.

Workup

  1. concentrationconcentrated
  2. additionThe concentrate is diluted with water and ethyl acetate
  3. customthe aqueous layer separated
  4. customfreeze dried

Sources & evidence

ORD record
ord-915df9fe53ee4297bacbfecf009e7cc4
Source dataset
uspto-grants-1993_06
Patent number
US05220021

Reaction notes

Loading…