反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
This compound was prepared in a manner analogous to Example 87 using diethyl (4-{[4-chloro-5-(trifluoromethyl)pyrimidin-2-yl]amino}-3-methoxybenzyl)phosphonate and 7-amino-4-(trans-4-hydroxycyclohexyl)-2-methyl-2,3-dihydro-1H-isoindol-1-one. Purification: ISCO Combi-flash RF system eluting with 0 to 5% MeOH in EtOAc. The pure product was dissolved in 1 mL of 12M HCl then concentrated in vacuo to afford the title compound as the HCl Salt: 1H NMR (400 MHz, DMSO-d6) δ10.60 (s, 1H), 9.10 (br. s., 1H), 8.37 (s, 1H), 7.43 (br. s., 1H), 7.31 (d, J=8.59 Hz, 1H), 7.07 (s, 1H), 6.92 (d, J=7.83 Hz, 1H), 4.48 (s, 2H), 3.92-4.05 (m, 7H), 3.44-3.56 (m, 1H), 3.23-3.35 (m, 2H), 3.06 (s, 3H), 1.92 (d, J=10.36 Hz, 2H), 1.54-1.75 (m, 4H), 1.23-1.33 (m, 2H), 1.19 (t, J=7.07 Hz, 6H). MS (ES+): m/z: 678.24 [MH+]. HPLC: tR=3.37 min (Micromass ZQ3: polar—5 min).
WORKUP
后处理
- customPurification
- washISCO Combi-flash RF system eluting with 0 to 5% MeOH in EtOAc
- dissolutionThe pure product was dissolved in 1 mL of 12M HCl
- concentrationthen concentrated in vacuo