反应详情

To a well stirred suspension of 125 g of 4-methylthiosemicarbazide and 165 g of β-chloropivalic acid in 500 ml of dioxane was added 186 g of phosphorus oxychloride at a rate which maintained the temperature below 60°. The reaction mixture was then heated at reflux until HCl evolution ceased (about 4 hrs). After cooling, the supernatant liquid was decanted from the plastic mass and 500 ml of water was added. With cooling, sodium hydroxide pellets were added until a pH of 10 was maintained. The resulting precipitate was collected, washed with water and air dried giving 216 g m.p. 91°-93°, (87%). Recrystallization from methylene chloride-ether gave the analytical sample, m.p. 93°-95°.

1. temperaturemaintained the temperature below 60°
2. temperatureThe reaction mixture was then heated
3. custom(about 4 hrs)
4. temperatureAfter cooling
5. customthe supernatant liquid was decanted from the plastic mass and 500 ml of water
6. additionwas added
7. temperatureWith cooling
8. additionsodium hydroxide pellets were added until a pH of 10
9. temperaturewas maintained
10. customThe resulting precipitate was collected
11. washwashed with water and air
12. customdried
13. customgiving 216 g m.p. 91°-93°, (87%)
14. customRecrystallization from methylene chloride-ether
15. customgave the analytical sample, m.p. 93°-95°