HRID656346

反应详情

EQUATION

反应方程式

HRID 656346 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

tert-Butyl (3S)-3-[((3S)-1-[(3-chloro-2-methylphenyl)sulfonyl]piperidin-3-ylamino)-carbonyl]-piperidine-1-carboxylate (10.0 mg, 200 μmol) was treated with 4.0 M of hydrogen chloride in 1,4-dioxane (0.5 mL) at rt for 1 h. The volatiles were removed in-vacuo and the residue was dissolved in acetonitrile (0.8 mL) and was treated with diisopropylethylamine (20.0 μL) and acetyl chloride (5.0 μL). The crude reaction mixture was diluted with MeOH (1.3 mL) and was adjusted to a pH of 2 using TFA and was purified by prep-HPLC to give the desired product. LCMS: (M+H)+=442.1/444.1.

WORKUP

后处理

  1. customThe volatiles were removed in-vacuo
  2. dissolutionthe residue was dissolved in acetonitrile (0.8 mL)
  3. additionwas treated with diisopropylethylamine (20.0 μL) and acetyl chloride (5.0 μL)
  4. customThe crude reaction mixture
  5. customwas purified by prep-HPLC