HRID2224079

反应详情

EQUATION

反应方程式

HRID 2224079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(7-Benzenesulfonyl-2,3-dihydro-benzo[1,4]oxazin-4-yl)-piperidine-1-carboxylic acid tert-butyl ester (0.111 g, 0.242 mmol) was dissolved in 5 mL ethyl alcohol and brought to reflux. To the solution was added ethanolic hydrogen chloride (2 mL of a 2N solution, 4.0 mmol) and reflux continued for 0.5 hours. The solution is concentrated to 1 mL and ethyl ether (10 mL) is added until a white precipitate is observed. Filtration gave 0.085 g (quantitative) of 7-benzenesulfonyl-4-piperidin-4-yl-3,4-dihydro-2H-benzo[1,4]oxazine hydrochloride as a white powder. MS: 359 (M+H)+, mp: 251.9-253.2° C.

WORKUP

后处理

  1. temperatureto reflux
  2. temperaturereflux
  3. concentrationThe solution is concentrated to 1 mL and ethyl ether (10 mL)
  4. additionis added until a white precipitate
  5. filtrationFiltration