反应 #895

ord-bbaa547034cb4578bce2648d1c091a1f

反应方程式

C[S-].[Na+]
sodium thiomethoxide
Clc1cc(Cl)nc(OCc2ccccc2)n1
4,6-dichloro-2-(phenylmethoxy)pyrimidine
CSc1cc(Cl)nc(OCc2ccccc2)n1
4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to react for 2 hours
  2. 2
    其他the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
  3. 3
    洗涤The organic layer was washed with aqueous saturated sodium chloride
  4. 4
    干燥dried over anhydrous sodium sulfate
  5. 5
    浓缩concentrated
  6. 6
    其他purified on a silica gel column

实验过程

Aqueous sodium thiomethoxide (15%, 2.75 g, 0.0059×1.0 mol) was added dropwise in 4,6-dichloro-2-(phenylmethoxy)pyrimidine (Compound No. II-26) (1.5 g, 0.0059 mol) dissolved in THF at room temperature. After allowed to react for 2 hours, the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, then purified on a silica gel column to obtain 4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine (Compound No. II-15) as an intermediate.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723412uspto-grants-1998_03