HRID1479935
反应详情
EQUATION
反应方程式
REACTANTS
反应物
HCID6228
N,N-Dimethylformamide
C3H7NO
HCID8471
Triethylamine
C6H15N
HCID15908
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide
C8H17N3
HCID78168
2,4(1H,3H)-Pyrimidinedione, 5-(hydroxymethyl)-
C5H6N2O3
HCID444972
Fumaric acid
C4H4O4
HCID2733084
Methanaminium, N-[(1H-benzotriazol-1-yloxy)(dimethylamino)methylene]-N-methyl-, hexafluorophosphate(1-) (1:1)
C11H16F6N5OP
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
5-(Hydroxymethyl)-1H-pyrimidine-2,4-dione (3.0 eq) was added to a mixture of fumaric acid (1.0 g, 1.0 eq), EDAC (or HBTU) (4.0 eq) and triethylamine (6.0 eq) in dichloromethane (or DMF) (50 mL). The mixture was stirred at 0° C. for 1 h and then at 20° C. overnight. The reaction was concentrated in vacuo to a residue and then purified by reverse-phase (C-18) liquid chromatography using water and acetonitrile as eluents to yield compound (6). MS (ESI): m/z 365.1 (M+H)+.
WORKUP
后处理
- customat 20° C.
- customovernight
- concentrationThe reaction was concentrated in vacuo to a residue
- custompurified by reverse-phase (C-18) liquid chromatography