HRID1768461

反应详情

EQUATION

反应方程式

HRID 1768461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. waitthe mixture was left
  2. customThe reaction was quenched with 1 drop of water
  3. washeluted with CH3CN/H2O with 0.1% TFA