反应详情

A mixture of 5% palladium on carbon (1 g.) and 2.0 g. (0.0066 mole) of the product of Procedure 1 in MeOH (50 ml.) was hydrogenated until H2 uptake ceased. The catalyst was removed and carbon disulfide (0.5 g. 0.0066 mole) was added. The solution was refluxed for 4 hrs. and stirred at room temperature for 16 hrs. The mixture was concentrated in vacuo and the residue suspended in H2O (50 ml.), and refluxed for 6 hrs., cooled, and 1.55 g. of solid collected by filtration. The solid was dissolved in dil. NaOH, treated with activated carbon, and reprecipitated with HOAc to give 1.18 g. of product, m.p. 232°-235°.

1. customThe catalyst was removed
2. temperatureThe solution was refluxed for 4 hrs
3. concentrationThe mixture was concentrated in vacuo
4. temperaturerefluxed for 6 hrs
5. temperature, cooled
6. filtrationof solid collected by filtration
7. dissolutionThe solid was dissolved in dil. NaOH
8. additiontreated with activated carbon
9. customreprecipitated with HOAc
10. customto give 1.18 g