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HRID629908

反应详情

EQUATION

反应方程式

HRID 629908 的结构方程式

REACTANTS

反应物

3
结构：[H-].[Na+]
HCID24758

Sodium hydride

HNa

结构：CN1C(=O)CNC1=O
HCID138851

2,4-Imidazolidinedione, 3-methyl-

C4H6N2O2

结构：Cn1c(=O)n(CC(C)(C)C)c2ccc([C@@H]3C[C@H]3COS(C)(=O)=O)nc21
HCID117702620

未命名化合物

PRODUCTS

生成物

1
结构：CN1C(=O)CN(C[C@@H]2C[C@H]2c2ccc3c(n2)n(C)c(=O)n3CC(C)(C)C)C1=O
HCID117702410

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

{(1R,2R)-2-[1-(2,2-Dimethylpropyl)-3-methyl-2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-5-yl]cyclopropyl}methyl methanesulfonate (31-5, 68 mg, 0.18 mmol, 1.0 equiv) was added to anhydrous DMF (0.92 mL) and cooled to 0° C. 3-Methylimidazolidine-2,4-dione (31-6, 105 mg, 0.92 mmol, 5.0 equiv) and NaH (37 mg, 0.92 mmol, 5.0 equiv, 60% dispersion in oil) were added sequentially and the resulting mixture was warmed to RT. After 18 h, LCMS showed complete consumption of 31-5. Purification by reverse-phase HPLC (10-100% 0.1% TFA in H2O:CH3CN) afforded 31-7 as a colorless oil. MS m/z (M+H): calculated=332.1969; observed=332.1971.

WORKUP

后处理

  1. temperaturethe resulting mixture was warmed to RT
  2. customconsumption of 31-5
  3. customPurification by reverse-phase HPLC (10-100% 0.1% TFA in H2O:CH3CN)