O-Cresol → HCID 66847074, compound

HRID 1980343Notes

Reaction equation

HRID 1980343 reaction equation
[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8].C1(C)C(O)=CC=CC=1>C1CCCCC1>[CH2:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8]

Participants

4

Reactant 2

HCID 335O-CresolHCID 342M-Cresol

Product 1

HCID 66847074HCID 66847074, compound

Reagents, catalysts & solvents 1

HCID 8078CyclohexaneSolvent2×

Procedure

The finished compositions were analyzed for amount of graft copolymer, amount of nylon in the graft copolymer and amount of free rubber (i.e., hydrogenated polymer or polymer adduct) using a coacervation procedure. In this procedure, 1.50 grams of composition were first dissolved in 30 ml. of m-cresol. Then, the resultant solution was diluted with 120 ml. of cyclohexane. The resultant suspension was then centrifuged to produce a large clear cyclohexane rich top layer and a small cresol rich lower layer. The top layer was removed by siphoning or decantation and then coagulated in 500 ml of methanol, filtered, washed in methanol, dried and weighed. The free rubber was obtained from this fraction by extracting the material with refluxing toluene for 48 hours. Then, 150 ml of an 81/19 cyclohexane/m-cresol mixture was added to the solution in the cresol-rich lower layer. The centrifugation and siphoning procedure was repeated and a second fraction was obtained. Subsequent fractions were obtained with 150 ml of 80/20, 79.5/20.5, 79/21, 78/22, 77/23, 76/24, 75/25 and 65/35 cyclohexane/m-cresol mixtures. All fractions were coagulated by adding them slowly to methanol and were collected on tared funnels. After washing with methanol, the samples were dried and weight of material was obtained.

Workup

  1. dissolutionIn this procedure, 1.50 grams of composition were first dissolved in 30 ml
  2. customThe top layer was removed
  3. filtrationfiltered
  4. washwashed in methanol
  5. customdried
  6. customThe free rubber was obtained from this fraction
  7. extractionby extracting the material with refluxing toluene for 48 hours
  8. additionThen, 150 ml of an 81/19 cyclohexane/m-cresol mixture was added to the solution in the cresol-rich lower layer
  9. customa second fraction was obtained

Sources & evidence

ORD record
ord-a878644d753b46c5b4195d24652d75f0
Source dataset
uspto-grants-1985_04
Patent number
US04508874

Reaction notes

Loading…