Phosphoric Acid → HCID 19438173, compound

HRID 2379254Notes

Reaction equation

HRID 2379254 reaction equation
[C:1]1([CH3:22])[CH:6]=[CH:5][C:4]([P:7]([C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=2)[C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[CH:3][CH:2]=1.[CH2:23]([I:25])[CH3:24].P(=O)(O)(O)O>C1(C)C=CC=CC=1>[I-:25].[CH2:23]([P+:7]([C:4]1[CH:5]=[CH:6][C:1]([CH3:22])=[CH:2][CH:3]=1)([C:15]1[CH:16]=[CH:17][C:18]([CH3:21])=[CH:19][CH:20]=1)[C:8]1[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=1)[CH3:24]

Participants

5

Reactant 3

HCID 1004Phosphoric AcidHCID 6340IodoethaneHCID 13956Phosphine, tris(4-methylphenyl)-

Product 1

HCID 19438173HCID 19438173, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
25 °C

Procedure

Into a 50 milliliter glass reactor equipped with a thermometer connected to a temperature controller, a heating mantle, a condenser and a magnetic stirring bar, is charged 5 gms (0.0164 mole) of tri-p-tolyl phosphine and 25 gms of toluene. The slurry is heated to 25° C., then 3 gms (0.0192 mole) of ethyl iodide is added. This reaction mass is heated to 60° C. and maintained for 14 hours, then cooled and the resulting phosphonium salt collected by filtration. After vacuum drying, there is obtained 6.85 gms of catalyst which has a melting point of 184°-187° C. and a chemical shift of 24.7 ppm (phosphoric acid reference).

Workup

  1. customInto a 50 milliliter glass reactor equipped with a thermometer
  2. temperatureThis reaction mass is heated to 60° C.
  3. temperaturemaintained for 14 hours
  4. temperaturecooled
  5. filtrationthe resulting phosphonium salt collected by filtration
  6. customAfter vacuum drying
  7. customthere is obtained 6.85 gms of catalyst which

Sources & evidence

ORD record
ord-3cf262f4a8684188ab1b9a6cf2ebebd4
Source dataset
uspto-grants-1994_11
Patent number
US05360886

Reaction notes

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