HRID1943654

反应详情

EQUATION

反应方程式

HRID 1943654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 5 ml flask, 3,4-dihydro-2H-pyrido[4,3-b][1,4]oxazine (30 mg, 0.220 mmol) was dissolved in tetrahydrofuran (3 ml). Diisopropylethylamine (0.153 ml, 0.878 mmol) was added and then stirred at 0□ for 10 minutes, and then 3,5-dichloro-4-hydroxy-benzenesulfonyl chloride (69 mg, 0.264 mmol) was added thereto and then stirred at 0□ for 1 hour. The reaction mixture was evaporated under reduced pressure. The residue was purified by column chromatography on silica eluting with a solvent of dichloromethane:ethyl acetate=1:2. The fractions containing the product were collected and evaporated to obtain the target compound 21 as pale-yellow solid (2.7 mg, 3.4%).

WORKUP

后处理

  1. stirringstirred at 0□ for 1 hour
  2. customThe reaction mixture was evaporated under reduced pressure
  3. customThe residue was purified by column chromatography on silica eluting with a solvent of dichloromethane
  4. additionThe fractions containing the product
  5. customwere collected
  6. customevaporated