2,4,6-Cycloheptatrien-1-one, 2-chloro- → 1073-38-7

Temperature

-70 °C

A solution of 2-chloro-2,4,6-cycloheptatrien-1-one [2.82 g, described by T. Nozoe et al., Proc. Japan Acad., 28, 483 (1952)] in ethanol (20 ml) is added dropwise to a suspension, cooled to -70° C., of sodium sulfhydrate (2.2 g) in ethanol (20 ml). The mixture is stirred at -70° C. for two hours, allowed to warm to room temperature and stirred at room temperature for one hour. The mixture is filtered and the filtrate is evaporated. The residue is suspended in water, the mixture is acidified to pH 2 with 10% hydrochloric acid and extracted with ethyl acetate. The organic extract is dried and evaporated. The residue is dissolved in benzene and subjected to chromatography on silica gel. The eluates are evaporated to give the title compound, mp 55° C.

1. temperatureto warm to room temperature
2. stirringstirred at room temperature for one hour
3. filtrationThe mixture is filtered
4. customthe filtrate is evaporated
5. extractionextracted with ethyl acetate
6. extractionThe organic extract
7. customis dried
8. customevaporated
9. dissolutionThe residue is dissolved in benzene
10. customThe eluates are evaporated

ORD record

ord-93f8fc4cedcc4464a1d9ab1fa3fa1031

Source dataset

uspto-grants-1979_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04152456