Phosphoric Acid → HCID 18958192, compound
Reaction equation
[C:1]1([CH3:22])[CH:6]=[CH:5][CH:4]=[C:3]([P:7]([C:15]2[CH:16]=[C:17]([CH3:21])[CH:18]=[CH:19][CH:20]=2)[C:8]2[CH:9]=[C:10]([CH3:14])[CH:11]=[CH:12][CH:13]=2)[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:15]1[CH:16]=[C:17]([CH3:21])[CH:18]=[CH:19][CH:20]=1)([C:3]1[CH:2]=[C:1]([CH3:22])[CH:6]=[CH:5][CH:4]=1)[C:8]1[CH:9]=[C:10]([CH3:14])[CH:11]=[CH:12][CH:13]=1)[CH3:24]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 40 °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 5.49 gms (0.0181 mole) of tri-m-tolyl phosphine and 25 gms of toluene. The slurry is heated to 40° C., then 3.38 gms (0.0217 mole) of ethyl iodide is added. This reaction mass is heated to 40° C. and maintained for 16 hours, then heated to 70° C. and maintained for 4 hours, then cooled to 30° C. and the resulting phosphonium salt collected by filtration. After vacuum drying, there is obtained 5.8 gms of catalyst which has a melting point of >250° C. and a chemcial shift of 25.7 ppm (phosphoric acid reference).
Workup
- customInto a 50 milliliter glass reactor equipped with a thermometer
- temperatureThis reaction mass is heated to 40° C.
- temperaturemaintained for 16 hours
- temperatureheated to 70° C.
- temperaturemaintained for 4 hours
- temperaturecooled to 30° C.
- filtrationthe resulting phosphonium salt collected by filtration
- customAfter vacuum drying
- customthere is obtained 5.8 gms of catalyst which
Sources & evidence
- ORD record
- ord-1c193d01c59d45cf86b524c8e6ee63aa
- Source dataset
- uspto-grants-1994_11
- Patent number
- US05360886
Reaction notes
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