反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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).
WORKUP
后处理
- customA three-necked flask equipped with a reflux condenser
- additionmixed for three minutes
- temperaturewas heated by immersion in an oil bath
- customadjusted to 85° C
- distillationwere distilled off
- customrecovered under reduced pressure
- distillationThen, a distillation under reduced pressure
- customheating at 100° C. to 108° C.
- distillationdistill it out under a reduced pressure of 533 Pa (4 mmHg)