Phosphine, 1H-inden-1-yldiphenyl- → HCID 178506783, compound

HRID 1387659Notes

Reaction equation

HRID 1387659 reaction equation
[CH:1]1([P:10]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.[Li:23]CCCC>CCOCC.CCCCCC>[C:11]1([P:10]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:1]2([Li:23])[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[CH:3]=[CH:2]2)[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

Participants

5

Reactant 2

HCID 12074547Phosphine, 1H-inden-1-yldiphenyl-HCID 178418339Butyllithium

Product 1

HCID 178506783HCID 178506783, compoundYield 87.3%

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 8058HexaneSolvent

Procedure

(1H-Inden-1-yl)diphenylphosphine (5.00 g, 16.65 mmol) was dissolved in a mixture of 60 mL of ether and 60 mL of hexane. n-BuLi (7.35 mL, 18.31 mmol) was added to the mixture within 10 minutes. After stirring overnight no precipitate appeared. Solvent was removed under reduced pressure leaving a waxy yellow residue. This residue was triturated with 120 mL of hexane for 15 minutes The hexane solution was decanted and the residue was dried under reduced pressure to give 4.45 g of off-white solid. Yield 87 percent.

Workup

  1. customSolvent was removed under reduced pressure
  2. customleaving a waxy yellow residue
  3. customThis residue was triturated with 120 mL of hexane for 15 minutes The hexane solution
  4. customwas decanted
  5. customthe residue was dried under reduced pressure

Sources & evidence

ORD record
ord-bee1d864e2a14632bb10c2aa51410d50
Source dataset
uspto-grants-2001_07
Patent number
US06268444B1

Reaction notes

Loading…