HRID18574
反应详情
EQUATION
反应方程式
REACTANTS
反应物
HCID81531
Diisopropylethylamine
C8H19N
2 次
HCID225209
1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1h-purine-8-carboxylic acid
C8H8N4O4
HCID9886157
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
C10H15F6N6OP
HCID17750340
1-(Propan-2-yl)piperidin-4-amine--hydrogen chloride (1/2)
C8H20Cl2N2
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
100 mg (0.45 mmol) 1,3-Dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purine-8-carboxylic acid were dissolved in 5 mL DMF. Subsequently 227 μl (1.35 mmol) DIPEA and 186.5 mg (0.495 mmol) HATU were added. After 1 h 105.6 mg (0.495 mmol) 1-isopropyl-piperidine-4-ylamine-dihydrochloride and 227 μl (1.35 mmol) DIPEA were added and the resulting mixture was stirred at room temperature for 4 h. The reaction mixture was concentrated and purified by preparative RP-HPLC (CH3CN/H2O gradient+0.05% formic acid) to give 1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purine-8-carboxylic acid (1-isopropyl-piperidin-4-yl)-amide as its formiate.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- custompurified by preparative RP-HPLC (CH3CN/H2O gradient+0.05% formic acid)