HRID481966
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 3-methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate (0.5 g), octylamine (0.5 mL) and m-chlorotoluene (3 mL) was refluxed for 2-3 h (until completion of the reaction; t.l.c.). Most of the solvents were removed by distillation and the residue was dispersed in a mixture of water (30 mL) and methanol (30 mL) and supplemented with NaOH 10% w/v in water (2 mL). The mixture was treated with charcoal, filtered, and the filtrate was adjusted to pH 6 with 1N HCl. The resulting precipitate was collected by filtration, washed with water and dried (yield: 0.29 g); m.p. 176°-179° C. (Compound 13).
WORKUP
后处理
- temperaturewas refluxed for 2-3 h (
- customuntil completion of the reaction
- customMost of the solvents were removed by distillation
- additionthe residue was dispersed in a mixture of water (30 mL) and methanol (30 mL)
- additionThe mixture was treated with charcoal
- filtrationfiltered
- filtrationThe resulting precipitate was collected by filtration
- washwashed with water
- customdried (yield: 0.29 g)