Phosphorus sulfide (P2S5) → HCID 20472108, compound

HRID 2296261Notes

Reaction equation

HRID 2296261 reaction equation
[CH2:1]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:2][CH:3]([CH3:5])[CH3:4].[P:13]12(SP3(SP(SP(S3)(S1)=S)(=S)[S:15]2)=S)=[S:14]>CCCCCC>[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][CH:3]([CH3:5])[CH3:4]

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 517982HCID 517982, compound

Product 1

HCID 20472108HCID 20472108, compound

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

iso-Pentyloxybenzene (Ib) and P4S10 (in a molar ratio of 10:1) were stirred for six hours at 150° C. under anhydrous conditions. The mixture was cooled, hexane was added, and the reaction flask was left for two days at 5° C. The resulting precipitate was recovered by filtration, washed with anhydrous hexane and dried. The yield of product was 27% of theory; after recrystallization from chloroform/petroleum ether it melted at 150°-2° 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 hexane
  4. customdried
  5. customafter recrystallization from chloroform/petroleum ether it melted at 150°-2° C
  6. customat room temperature

Sources & evidence

ORD record
ord-a135a0778ee94ec899292e4dafd231f4
Source dataset
uspto-grants-1984_01
Patent number
US04428889

Reaction notes

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