HRID1180377
反应详情
EQUATION
反应方程式
REACTANTS
反应物
HCID8471
Triethylamine
C6H15N
HCID143452
tert-Butyl piperazine-1-carboxylate
C9H18N2O2
HCID236361
4-[hydroxy(phenyl)methyl]benzoic acid
C14H12O3
HCID516892
Sodium Bicarbonate
CHNaO3
HCID9886157
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
C10H15F6N6OP
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of the crude compound of 4-[hydroxy(phenyl)methyl]benzoic acid (1.51 g, 6.6 mmol) in DMF (33 mL) was added tert-butyl piperazine-1-carboxylate (1.23 g, 6.6 mmol), triethylamine (3.7 mL, 26.5 mmol) and HATU (2.51 g, 6.6 mmol). The mixture was aged for 3 hours under a nitrogen atmosphere and was then poured into a saturated aqueous solution of NaHCO3. The resulting mixture was extracted 3 times with ethyl acetate. The combined organic layers were washed with brine, dried and evaporated to a solid which was stirred in ethyl acetate at room temperature for 2 hours. The title compound was then recovered by filtration as a white solid.
WORKUP
后处理
- extractionThe resulting mixture was extracted 3 times with ethyl acetate
- washThe combined organic layers were washed with brine
- customdried
- customevaporated to a solid which
- filtrationThe title compound was then recovered by filtration as a white solid