HRID1929337

反应详情

EQUATION

反应方程式

HRID 1929337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

a solution of 5 g of 2,4,6-trichloro-1,3,5-triazine in 5.5 cm3 of N,N-dimethylformamide is stirred for about 3 hours at a temperature close to 20° C. A white precipitate forms. A solution of 5 g of 1-(2,6-dichlorophenyl)-ethanol in 72 cm3 of dichloromethane is added dropwise without exceeding 25° C. After about 48 hours at a temperature close to 20° C., the suspension is solubilized by adding 150 cm3 of dichloromethane. The solution obtained is washed five times with 40 cm3 of water, then dried over magnesium sulphate, filtered and concentrated under reduced pressure. After filtration of the residue on 100 cm3 of silica [eluent: cyclohexane/ethyl acetate (75/25 by volume)], we obtain 5.5 g of 1,3-dichloro-2-(1-chloroethyl)benzene in the form of a colorless oil, which has the following characteristics:

WORKUP

后处理

  1. customclose to 20° C
  2. customwithout exceeding 25° C
  3. customAfter about 48 hours at a temperature close to 20° C.
  4. customThe solution obtained
  5. washis washed five times with 40 cm3 of water
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. filtrationAfter filtration of the residue on 100 cm3 of silica [eluent: cyclohexane/ethyl acetate (75/25 by volume)], we