反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of N-[2-[[[5-[(dimethylamino)methyl]-4-methyl-2-furanyl]methyl]thio]ethyl]-N'-methyl-2-nitro-1,1-ethenediamine (6.465 g) in water (25 ml) was added bismuth citrate (7.84 g) and the mixture heated at 100° for 4 hours. The suspension was filtered and the residue washed well with water then ethanol and dried to give a solid consisting of unchanged bismuth citrate (2.448 g) which was discarded. The combined filtrate and washings were evaporated to dryness with the aid of methanol (3×50 ml) then ethanol (2×50 ml). The residue was mixed with cold ethanol (70 ml) and triturated to a fine cream which was filtered off, washed with ethanol (4×5 ml) and then ether and dried to give the title compound (9.187 g).
WORKUP
后处理
- temperaturethe mixture heated at 100° for 4 hours
- filtrationThe suspension was filtered
- washthe residue washed well with water
- dry with materialethanol and dried
- customto give a solid
- customThe combined filtrate and washings were evaporated to dryness with the aid of methanol (3×50 ml)
- additionThe residue was mixed with cold ethanol (70 ml)
- customtriturated to a fine cream which
- filtrationwas filtered off
- washwashed with ethanol (4×5 ml)
- dry with materialether and dried