Carbon Tetrachloride → HCID 22154346, compound

HRID 868002Notes

Reaction equation

HRID 868002 reaction equation
[C:1]([Cl:5])([Cl:4])([Cl:3])[Cl:2].[C:6]1([P:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>C1COCC1.CCCCCC>[C:1]([Cl:5])([Cl:4])([Cl:3])[Cl:2].[C:19]1([P:12]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

Participants

5

Reactant 2

HCID 5943Carbon TetrachlorideHCID 11776Triphenylphosphine

Product 1

HCID 22154346HCID 22154346, compound

Reagents, catalysts & solvents 2

HCID 8028TetrahydrofuranSolventHCID 8058HexaneSolvent

Procedure

A solution of D-2 (304 mg), carbon tetrachloride (0.19 ml, 2 mmole), triphenylphosphine (524 mg), and TEA (0.28 ml) in dry THF (5 ml) is stirred under argon for 4 days. The reaction mixture is diluted with hexane (5 ml), filtered through a short silica column (elution with ethyl acetate/hexane, 1:1), and the filtrate concentrated. Chromatography of the residue on silica gel (elution with hexane/ethylacetate, 2:1) delivers D-3 as a solid.

Workup

  1. filtrationfiltered through a short silica column (elution with ethyl acetate/hexane, 1:1)
  2. concentrationthe filtrate concentrated

Sources & evidence

ORD record
ord-49b0bab1f6c247259bb3ba1a1a86d6b0
Source dataset
uspto-grants-1988_10
Patent number
US04777286

Reaction notes

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