HRID2225279

反应详情

EQUATION

反应方程式

HRID 2225279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The entirety of tert-butyl(1R,3R,4S)-3-((S)-1-hydroxy-2-methylpropyl)-4-(2-(3-(trifluoromethyl)benzamido)acetamido)cyclohexylcarbamate prepared in previous Step (1 eq) in CH2Cl2 (20 mL) was added TFA (4 mL) at RT. The reaction was stirred for 5 h and concentrated in vacuo. The residue was partitioned between 1N NaOH (30 mL) and EtOAc (40 mL). The aqueous layer was extracted with EtOAc (2×50 mL) and the organic phases were combined, washed with brine (25 mL), dried (Na2SO4), filtered, and concentrated in vacuo to give N-(2-((1S,2R,4R)-4-amino-2-((S)-1-hydroxy-2-methylpropyl)cyclohexylamino)-2-oxoethyl)-3-(trifluoromethyl)benzamide. MS found: (M+H)+=416.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. customThe residue was partitioned between 1N NaOH (30 mL) and EtOAc (40 mL)
  3. extractionThe aqueous layer was extracted with EtOAc (2×50 mL)
  4. washwashed with brine (25 mL)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo