Hydrochloric Acid → HCID 22222996, compound

A 500 mL round bottom flask equipped with a mechanical stirrer was charged with 18.9 g (0.15 mol) 3-cyclohexene-1-carboxylic acid, and 300 mL of ether. 132 mL of hexylithium (2.5 M solution in hexane, 0.33 mol) was slowly added to above mixture in ice bath over 40 min. After the above mixture was reacted at 0° C. for 30 minutes, the reaction mixture was warmed to room temperature. The mixture is slowly added into a vigorously stirred mixture of 27 mL (0.32 mol) of concentrated HCl and 400 mL of water. The organic phase is separated, and aqueous phase is extracted with 3×150 mL of ether, the combined organic solution is dried over sodium sulfate, and the solution is evaporated and distilled to give pure product.

1. customA 500 mL round bottom flask equipped with a mechanical stirrer
2. customAfter the above mixture was reacted at 0° C. for 30 minutes
3. customThe organic phase is separated
4. extractionaqueous phase is extracted with 3×150 mL of ether
5. dry with materialthe combined organic solution is dried over sodium sulfate
6. customthe solution is evaporated
7. distillationdistilled
8. customto give pure product

ORD record

ord-0a967f0552dc4ab6a84b528b3950c2a6

Source dataset

uspto-grants-2006_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07018559B2