Phosphoric Acid → HCID 18958205, compound

HRID 2379255Notes

Reaction equation

HRID 2379255 reaction equation
[C:1]1([CH3:22])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[P:7]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:21])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14].[CH2:23]([I:25])[CH3:24].P(=O)(O)(O)O>C1(C)C=CC=CC=1>[I-:25].[CH2:23]([P+:7]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:21])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[CH3:22])[CH3:24]

Participants

5

Reactant 3

HCID 1004Phosphoric AcidHCID 6340IodoethaneHCID 80271Tri-o-tolylphosphine

Product 1

HCID 18958205HCID 18958205, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
27 °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-o-tolyl phosphine and 23 gsm of toluene. The slurry is heated to 27° C. then 3.08 gms (0.0197 mole) of ethyl iodide is added. This reaction mass is heated to 70° C. and maintained for 15 hours, then cooled to 26° C. and the resulting phosphonium salt collected by filtration. The salt is washed with 6 gms of toluene dried. There is obtained 1.6 gms of catalyst which has a melting point of 247°-250° C. and a chemcial shift of 28.5 ppm (phosphoric acid reference).

Workup

  1. customInto a 50 milliliter glass reactor equipped with a thermometer
  2. temperatureThis reaction mass is heated to 70° C.
  3. temperaturemaintained for 15 hours
  4. temperaturecooled to 26° C.
  5. filtrationthe resulting phosphonium salt collected by filtration
  6. washThe salt is washed with 6 gms of toluene
  7. customdried
  8. customThere is obtained 1.6 gms of catalyst which

Sources & evidence

ORD record
ord-45802307e4dd46baa906e53f58c95a14
Source dataset
uspto-grants-1994_11
Patent number
US05360886

Reaction notes

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