ChemicalBook CAS DataBase List 1-CYCLOHEXEN-1-YL TRIFLUOROMETHANE-

1-CYCLOHEXEN-1-YL TRIFLUOROMETHANE- synthesis

8synthesis methods

Product Name:1-CYCLOHEXEN-1-YL TRIFLUOROMETHANE-
CAS Number:28075-50-5
Molecular formula:C7H9F3O3S
Molecular Weight:230.2

1493-13-6 Synthesis

1493-13-6
629 suppliers
$12.00/5g

108-94-1 Synthesis

108-94-1
546 suppliers
$12.00/50g

28075-50-5
38 suppliers
$45.00/10mg

Yield: 55%

Reaction Conditions:

Stage #1:cyclohexanone with lithium diisopropyl amide in tetrahydrofuran at 20; for 2 h;
Stage #2:trifluorormethanesulfonic acid in tetrahydrofuran at 20; for 9 h;

Steps:

1
First of all on the preparation of the LDA. The second ispropyl amine (9.8 ml, 69 . 9mmol) by adding 90 ml of water in the THF, -78 °C adding n-BuLi 41 ml (1.7N, 70mmol), after adding system temperature to 0 °C reaction 15min. Then the system as regards the -78 °C lower, the prepared LDA is a light yellow THF solution. For added LDA in DMPU 21 ml, and slowly drips into the compound N (cyclohexanone) (6 ml, 57 . 9mmol) THF solution of 50 ml, at this temperature the reaction 2h. After the solution is dripped slowly into three fluoro sulfonate (22g, 61.6mmol) of THF solution (60 ml), after dropping system at this temperature to continue the reaction 9h. After the reaction, the reaction solution directly silica gel mixes the type column chromatographic analysis (petroleum ether: ethyl acetate=20:1), to obtain a light yellow oil of very small viscosity 8.6g. The product is easy to deteriorate, immediately proceed with the next step of the reaction. Yield: 55%

References:

Fudan University;Shao, Liming;Chen, Jian;Yang, Xicheng;Yu, Mingcheng;Xiao, Li;Li, Wei;Xie, Qiong CN106278994, 2017, A Location in patent:Paragraph 0081; 0082; 0083; 0084; 0085

358-23-6 Synthesis