HRID1853463

反应详情

EQUATION

反应方程式

HRID 1853463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyl(R)-1-(4-hydroxycyclohexyl)ethylcarbamate (4.49 g, 18.45 mmol) was dissolved in dichloromethane (25 mL) and cooled to 0° C. under nitrogen. HCl 2M in Ether (27.68 mL of 2 M, 55.35 mmol) was added and the reaction allowed to warm slowly to ambient temperature for 18 hours. The reaction mixture was concentrated in vacuo. The crude mixture was dissolved in MeOH (25 mL). MP-Carbonate was added (11.75 g, 36.90 mmol) and the reaction mixture was stirred for 3 hours. The resin was filtered and the mother liquors were concentrated to dryness to afford the title compound as an off white solid (2.39 g, 90% yield).

WORKUP

后处理

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionThe crude mixture was dissolved in MeOH (25 mL)
  4. additionMP-Carbonate was added (11.75 g, 36.90 mmol)
  5. filtrationThe resin was filtered
  6. concentrationthe mother liquors were concentrated to dryness