HRID1295557

反应详情

EQUATION

反应方程式

HRID 1295557 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Methyl-3,4-dihydro-2H-benzo[1,4]oxazine (1.49 g, 10 mmol) was dissolved in dichloromethane (50 mL) and treated with triethylamine (1.14 g, 11 mmol) followed by the dropwise addition of methanesulfonyl chloride (1.26 g, 11 mmol). The mixture was stirred at ambient temperature for 18 h then evaporated to dryness under reduced pressure. The residue was partitioned between ethyl acetate and saturated aqueous NaHCO3. The phases were separated and the organic phase washed with water, saturated brine, dried (MgSO4) and evaporated to dryness under reduced pressure to give the title compound (2.09 g, 93%) as a brown solid.

WORKUP

后处理

  1. customthen evaporated to dryness under reduced pressure
  2. customThe residue was partitioned between ethyl acetate and saturated aqueous NaHCO3
  3. customThe phases were separated
  4. washthe organic phase washed with water, saturated brine
  5. dry with materialdried (MgSO4)
  6. customevaporated to dryness under reduced pressure