Triethoxysilane → 4,4-Bis(trifluoromethanesulfonyl)butyltriethoxysilane

Participants

Reaction Steps

A three-necked flask equipped with a reflux condenser and having a volume of 100 ml was charged under nitrogen atmosphere with each of 100.2 g (0.313 mol) of 1,1-bis(trifluoromethanesulfonyl)-3-butene (hereinafter abbreviated as BTSB), 69.8 g of toluene, 11.7 mg (0.0001 parts by mass relative to BTSB) of dichloro(1,5-cyclooctadiene)platinum (II) (made by Tokyo Chemical Industry Co., Ltd.), and 155.0 g (155 parts by mass relative to BTSB) of triethoxysilane (made by Tokyo Chemical Industry Co., Ltd.). After that, under nitrogen atmosphere, it was stirred and mixed for three minutes. Then, the reaction was conducted for 11 hours, while this flask was heated by immersion in an oil bath adjusted to 85° C. After the termination of the reaction, triethoxysilane and toluene were distilled off and recovered under reduced pressure. Then, a distillation under reduced pressure was conducted to carry out a heating at 100° C. to 108° C. and distill it out under a reduced pressure of 533 Pa (4 mmHg), thereby obtaining 98.8 g of 4,4-bis(trifluoromethanesulfonyl)butyltriethoxysilane (hereinafter abbreviated as BTSB-TES).

Provenance & Evidence