HRID1893202

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID2774597

3-Fluoro-4-methylbenzylamine

C8H10FN

结构：COC(=O)c1nc2n(c(=O)c1OS(C)(=O)=O)[C@H](C)CCC[C@H]2N(C)C(=O)C(=O)N(C)C

HCID87535816

未命名化合物

PRODUCTS

生成物

结构：Cc1ccc(CNC(=O)c2nc3n(c(=O)c2O)[C@H](C)CCC[C@H]3N(C)C(=O)C(=O)N(C)C)cc1F

HCID54748167

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID679

Dimethyl sulfoxide

C2H6OS

CONDITIONS

反应条件

温度: 100 °C

PROCEDURE

实验过程

The trans-rac-methyl 10-[[(dimethylamino)(oxo)acetyl](methyl)amino]-6-methyl-3-[(methylsulfonyl)oxy]-4-oxo-4,6,7,8,9,10-hexahydropyrimido[1,2-a]azepine-2-carboxylate from Step 10 (50 mg) was dissolved in DMSO (2 mL) and 4-methyl-3-fluorobenzylamine (0.1 mL) added. The resulting mixture was heated at 100° C. for 30 minutes. As determined by LC-MS, there was complete conversion to product which was purified by reverse phase Gilson chromatography: 1H NMR (400 MHz, CDCl3) δ 9.46 (br s, 1H), 7.05 (m, 3H), 5.96 (m, 1H), 5.56 (br s, 1H), 4.47 (qd, J=6.8, 14.5 Hz, 2H), 3.02 (s, 3H), 2.99 (s, 3H), 2.94 (s, 3H), 2.21 (s, 3H), 1.61-2.24 (m, 6H), 1.47 (d, J=7.5 Hz, 3H). ES MS M+1=487.8.

WORKUP

后处理

customwas purified by reverse phase Gilson chromatography