m-Chloroperbenzoic acid → HCID 22222980, compound

A 500 mL round bottom flask equipped with a stirrer bar was charged with 22.4g (0.10 mol) 3-(2-ethylhexoxymethyl)cyclohexene, and 50 mL of methylene chloride. m-Chloroperbenzoic acid (28.3 g, 85% in purity; 0.138 mol) in methylene chloride (200 mL) was added dropwise to above mixture over 1 hr in an ice bath. After the above mixture was reacted at room temperature overnight, the reaction mixture was filtered. The solid was washed with hexane (3×30 mL). The precipitate was filtered, 50 mL of hexane was added into filtrate to further precipate m-chlorobenzoic acid. The solid was filtered and washed with hexane (2×20 mL). The solvent was evaporated and the residue distilled to give pure product.

1. customA 500 mL round bottom flask equipped with a stirrer bar
2. customAfter the above mixture was reacted at room temperature overnight
3. filtrationthe reaction mixture was filtered
4. washThe solid was washed with hexane (3×30 mL)
5. filtrationThe precipitate was filtered
6. addition50 mL of hexane was added into filtrate to further precipate m-chlorobenzoic acid
7. filtrationThe solid was filtered
8. washwashed with hexane (2×20 mL)
9. customThe solvent was evaporated
10. distillationthe residue distilled
11. customto give pure product

ORD record

ord-4ce279f9c0364f05961b7cf8afbf5a37

Source dataset

uspto-grants-2006_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07018559B2