m-Chloroperbenzoic acid → HCID 19823850, compound

Temperature

0 °C

A solution of m-chloroperbenzoic acid (1.75 g) in dichloromethane (50 ml) was added over 30 minutes to a stirred solution of N,N-dimethyl-1-[1-(4-chlorophenyl)cyclobutyl]-4-methylthiobutylamine (2.4 g prepared in a similar manner to that described in Example 187) in dichloromethane (50 ml) at 0° C. The mixture was stirred at 0° C. for 11/2 hours and then kept at <5° C. overnight. The resulting solution was washed with 2N sodium hydroxide solution then brine and then dried and evaporated to give an oil which was treated with petroleum ether (b.p. 40°-60° C.). The resulting mixture was filtered and the filtrate evaporated to give a residue which was dissolved in 2N hydrochloric acid. The solution was washed with ether, basified and extracted with ether. The extracts were dried and evaporated to give N,N-dimethyl-1-[1-(4-chlorophenyl)-cyclobutyl]-4-methylsulphinylbutylamine as an oil the boiling point of which was not determined.

1. customprepared in a similar manner to that
2. customat 0° C
3. waitkept at <5° C. overnight
4. washThe resulting solution was washed with 2N sodium hydroxide solution
5. dry with materialbrine and then dried
6. customevaporated
7. customto give an oil which
8. filtrationThe resulting mixture was filtered
9. customthe filtrate evaporated
10. customto give a residue which
11. washThe solution was washed with ether
12. extractionextracted with ether
13. customThe extracts were dried
14. customevaporated

ORD record

ord-a1b06b51f8ca479b876601ef66c7c481

Source dataset

uspto-grants-1991_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05047432