Phosphorus sulfide (P2S5) → HCID 20472105, compound

HRID 2296259Notes

Reaction equation

HRID 2296259 reaction equation
[CH2:1]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH3:5].[P:13]12(SP3(SP(SP(S3)(S1)=S)(=S)[S:15]2)=S)=[S:14]>C1(C)C=CC=CC=1>[CH2:1]([O:6][C:7]1[CH:8]=[CH:9][C:10]([P:13](=[S:15])=[S:14])=[CH:11][CH:12]=1)[CH2:2][CH2:3][CH2:4][CH3:5]

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 16298Pentyl phenyl ether

Product 1

HCID 20472105HCID 20472105, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

n-Pentyloxybenzene (Ia) and P4S10 (in a molar ratio of 10:1) were stirred for six hours at 150° C. under anhydrous conditions. The mixture was cooled, toluene was added, and the reaction flask was left for two days at 5° C. The resulting precipitate was recovered by filtration, washed with anhydrous ether and dried. The yield of product was 46% of theory; after recrystallization from chloroform/petroleum ether it melted at 144°-6° C. Its solubility in tetrahydrofuran was found to be 5 gms/100 ml at room temperature.

Workup

  1. temperatureThe mixture was cooled
  2. filtrationThe resulting precipitate was recovered by filtration
  3. washwashed with anhydrous ether
  4. customdried
  5. customafter recrystallization from chloroform/petroleum ether it melted at 144°-6° C
  6. customat room temperature

Sources & evidence

ORD record
ord-f3182b5a99be42cdac04ce68d04eadfc
Source dataset
uspto-grants-1984_01
Patent number
US04428889

Reaction notes

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