HRID1529530

反应详情

EQUATION

反应方程式

HRID 1529530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of tert-butyl-2-amino-2-phenylacetate (1.34 g, 6.45 mmol) and methyl 3-(chlorosulfonyl)benzoate (1.53 g, 6.51 mmol) in tetrahydrofuran (15 mL) was added triethylamine (0.90 mL, 6.45 mmol) in one portion at ambient temperature. The reaction mixture was stirred for 30 minutes, after which time, the reaction mixture was concentrated under reduced pressure and partitioned between ethyl acetate (30 mL) and 10% citric acid solution (10 mL). The resulting organic phases were dried over magnesium sulfate and concentrated under reduced pressure to yield a crude solid. The solid was triturated in diethyl ether (5 mL) and cold methanol (5 mL) to yield the title compound as a white solid (1.13 g, 43%).

WORKUP

后处理

  1. concentrationafter which time, the reaction mixture was concentrated under reduced pressure
  2. custompartitioned between ethyl acetate (30 mL) and 10% citric acid solution (10 mL)
  3. dry with materialThe resulting organic phases were dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto yield a crude solid
  6. customThe solid was triturated in diethyl ether (5 mL)