HRID1768461
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 25 mg (0.07 mmol) of 1-9 in 1 mL of DMF was added a small amount of MeI and NaH (60% suspension in oil) and the mixture was left to stir for 15 h at room temperature. The reaction was quenched with 1 drop of water and loaded directly onto a RP HPLC and eluted with CH3CN/H2O with 0.1% TFA to provide 2-1 as a white solid. Data for 2-1: 1HNMR (500 MHz, CDCl3) δ 7.4-7.2 (m, 5H), 7.1-6.9 (m, 3H), 6.4 (s, 1H), 4.8 (d, 1H), 4.7 (d, 1H), 4.45 (d, 1H), 4.35 (d, 1H), 3.4 (s, 3H), 2.8 (s, 6H) ppm. HRMS (MS) calc'd M+H for C21H22F2N2O2: 373.1722. Found: 373.1722.
WORKUP
后处理
- waitthe mixture was left
- customThe reaction was quenched with 1 drop of water
- washeluted with CH3CN/H2O with 0.1% TFA