HRID13009

反应详情

EQUATION

反应方程式

HRID 13009 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[(1S,2R)-2-hydroxy-2-(3-methoxyphenyl)-1-methylethyl]carbamate (317 mg, 1.13 mmol) in dichloromethane (3 ml) was added water (3 ml), and TFA (5 ml), so that a clear solution has been obtained. The mixture was stirred at r.t. for 1 h, than poured into water (30 ml). The aqueous layer was washed with dichloromethane (30 ml), and made alkaline (pH≈10) by addition of 10 N aqueous NaOH. Brine (20 ml) was added, and the solution was extracted with dichloromethane (3×30 ml). The extracts were dried with Na2SO4, and the solvent was removed under reduced pressure to afford the subtitle compound as colourless oil. Yield 179 mg (88%).

WORKUP

后处理

  1. customso that a clear solution has been obtained
  2. washThe aqueous layer was washed with dichloromethane (30 ml)
  3. additionby addition of 10 N aqueous NaOH
  4. additionBrine (20 ml) was added
  5. extractionthe solution was extracted with dichloromethane (3×30 ml)
  6. dry with materialThe extracts were dried with Na2SO4
  7. customthe solvent was removed under reduced pressure