HRID484117

反应详情

EQUATION

反应方程式

HRID 484117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture heated at 100° for 4 hours
  2. filtrationThe suspension was filtered
  3. washthe residue washed well with water
  4. dry with materialethanol and dried
  5. customto give a solid
  6. customThe combined filtrate and washings were evaporated to dryness with the aid of methanol (3×50 ml)
  7. additionThe residue was mixed with cold ethanol (70 ml)
  8. customtriturated to a fine cream which
  9. filtrationwas filtered off
  10. washwashed with ethanol (4×5 ml)
  11. dry with materialether and dried