HCID 19995068, compound → HCID 131716979, compound

HRID 2248846Notes

Reaction equation

HRID 2248846 reaction equation
[CH3:1][C:2]1[C:7]([OH:8])=[C:6]([CH3:9])[C:5]([CH3:10])=[C:4]([C:11]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)([CH3:13])[CH3:12])[C:3]=1[CH3:21].CN([Si:29](N(C)C(N(C)C)=O)(C)C)C(N(C)C)=O>C1(C)C=CC=CC=1>[SiH4:29].[CH3:9][C:6]1[C:7]([OH:8])=[C:2]([CH3:1])[C:3]([CH3:21])=[C:4]([C:11]([C:14]2[CH:15]=[CH:16][C:17]([OH:20])=[CH:18][CH:19]=2)([CH3:13])[CH3:12])[C:5]=1[CH3:10]

Participants

4

Reactant 2

HCID 19995068HCID 19995068, compoundHCID 131712658HCID 131712658, compound2×

Product 1

HCID 131716979HCID 131716979, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent3×

Conditions

Temperature
78 °C

Procedure

There was added 9.4391 grams (0.03367 mols) of tetramethylbisphenol-A in increments of 4.72 grams, 2.36 grams and 2.35 grams at half hour intervals using 10 ml dry toluene to transfer each addition to 7.82 grams (0.03367 mols) of a 50% by weight toluene solution of bis(trimethylureido)dimethyl silane maintained under a nitrogen blanket at a temperature of 78° C. The final solution had about 27% by weight solids. The temperature of the resulting solution was raised to 120° C. one hour after the final tetramethylbisphenol-A addition to maintain the toluene solution under reflux . The reaction was monitored by GPC. The mixture was refluxed for an additional hour. A poly(tetramethylbisphenol-A monosiloxane) was obtained having a MWw of 17,800. After the removal of some toluene to increase the percent solids level, additional bisuriedo silane was added to provide a 7% excess. The reaction was left at reflux for two hours and an additional 2.35 millimoles of bisuriedo silane was added to provide a 14% excess silane. The reaction was continued for two hours diluted with toluene and then cooled slightly prior to precipitation in isopropanol. There was obtained a polymer having MWw of 56,500 and MWn of 32,900 by GPC.

Workup

  1. temperatureThe temperature of the resulting solution was raised to 120° C. one hour
  2. temperatureunder reflux
  3. temperatureThe mixture was refluxed for an additional hour

Sources & evidence

ORD record
ord-55fda685e86d404481bf53556e5b6efb
Source dataset
uspto-grants-1991_08
Patent number
US05041514

Reaction notes

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