Trimethylolpropane → HCID 22910808, compound

HRID 620062Notes

Reaction equation

[CH2:1]([C:3]([CH2:8][OH:9])([CH2:6][OH:7])[CH2:4][CH3:5])[OH:2].[C:10]1(=[O:17])[O:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1>CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-].[Ti+4]>[CH2:1]([C:3]([CH2:8][OH:9])([CH2:6][OH:7])[CH2:4][CH3:5])[OH:2].[C:10]1(=[O:17])[O:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1

Participants

Conditions

Temperature: 180 °C

Procedure

The same reactor as used in Referential Example 1 was charged with 134 parts (1 mole) of trimethylolpropane, 684 parts (6 moles) of epsilon-caprolactone and 0.04 part of tetrabutyl titanate, and the temperature of the mixture was raised to 180° C. in an atmosphere of nitrogen. The mixture was maintained at this temperature for 6 hours to give a 1:6 (by mole) trimethylolpropane/epsilon-caprolactone adduct. The temperature was then lowered to 90° C., and 936 parts of tetraethyl silicate (the equivalent ratio of tetraethyl silicate to hydroxyl groups=1.5) and 5.3 parts of tetrabutyl titanate were additionally fed, and the mixture was heated at 110° to 120° C. until the distillation of ethanol ceased (3 hours) to give a tetraethoxysilane-modified resin. This resin is designated as compound (C-2-3).

Workup

temperatureThe mixture was maintained at this temperature for 6 hours

Sources & evidence

ORD record: ord-c771f4c4622d4a6f876bb112a122aab5
Source dataset: uspto-grants-1989_04
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04818790

Reaction notes

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