HRID1408613

反应详情

EQUATION

反应方程式

HRID 1408613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Pd(PPh3)2Cl2 (10 mg) in a 10 mL tube under Ar was treated sequentially with 2′-amino-6-bromo-1′-methyl-2-phenylspiro[chroman-4,4′-imidazol]-5′(1′H)-one (20 mg, 0.052 mmol) in 1,4-dioxane (1 mL), Cs2CO3 (2 N, 0.3 mL) and phenylboronic acid (16 mg, 0.1 mmol). The mixture was heated under microwave at 120° C. for 30 minutes. The reaction mixture was concentrated in vacuo to give the residue, which was purified by preparative TLC and then by preparative HPLC to give pure 2′-amino-1′-methyl-2,6-diphenylspiro-[chroman-4,4′-imidazol]-5′(1′H)-one (1.55 mg, 5%). 1H-NMR (MeOD): 2.42 (m, 1H), 2.61 (m, 1H), 3.27 (s, 3H), 5.83 (d, 1H), 7.10 (d, 1H), 7.29 (m, 1H), 7.40 (m, 5H), 7.59 (m, 5H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customto give the residue, which
  3. customwas purified by preparative TLC