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
30 g of 4-hydroxyphenyl diphenylsulfonium nonafluoro-n-butanesulfonate was dissolved in 300 g of dichloromethane in a reaction flask, in which the atmosphere was replaced with nitrogen. 17.9 g of n-butanesulfonyl chloride and 10.5 g of triethylamine were added in this order. The mixture was stirred for 20 minutes at room temperature. After the addition of 100 g of ion-exchanged water, the mixture was transferred to a separatory funnel, shaken, and allowed to stand still. The water layer was removed. After the addition of 300 ml of distilled water, the solution was shaken and allowed to stand still. The water layer was removed. The resulting dichloromethane solution was dried using anhydrous magnesium sulfate and filtered. After evaporating dichloromethane from the dichloromethane solution, the residual liquid was dried under reduced pressure to obtain 26.7 g of 4-n-butanesulfonyloxyphenyl diphenylsulfonium nonafluoro-n-butanesulfonate. This compound is indicated as “acid generator (A-1)”.
WORKUP
后处理
- customthe mixture was transferred to a separatory funnel
- stirringshaken
- customThe water layer was removed
- additionAfter the addition of 300 ml of distilled water
- stirringthe solution was shaken
- customThe water layer was removed
- dry with materialThe resulting dichloromethane solution was dried
- filtrationfiltered
- customAfter evaporating dichloromethane from the dichloromethane solution
- customthe residual liquid was dried under reduced pressure