反応 #51621

反応方程式

NaH

cyclohexanol

2-chloro-6,7-dimethoxyquinoxaline

→

solid

2,7-Bis-cyclohexyloxy-6-methoxy-quinoxaline

溶媒

DMF

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction is stirred for 15 minutes at room temperature, at 90° C. for 2 hours
2. 2
   workup.WAITat 110° C. for 1 hour
3. 3
   温度The mixture is cooled
4. 4
   その他quenched with H2O
5. 5
   その他partition between EtOAc/H2O
6. 6
   洗浄The organic layer is washed with H2O and brine
7. 7
   乾燥dried (MgSO4)
8. 8
   その他chromatographed (10% EtOAc/hexanes)

実験手順

To a DMF solution (5 mL) of NaH (0.32 g, 8 mmol) under argon, cyclohexanol (0.7 mL. 6.7 mmol) is added dropwise. The mixture is stirred at room temperature for 25 minutes, then 2-chloro-6,7-dimethoxyquinoxaline is added portionwise. The reaction is stirred for 15 minutes at room temperature, at 90° C. for 2 hours, and at 110° C. for 1 hour. The mixture is cooled, quenched with H2O, and partition between EtOAc/H2O. The organic layer is washed with H2O and brine, dried (MgSO4), and chromatographed (10% EtOAc/hexanes) to provide a waxy white solid (m.p. 75-78° C.). Anal. Calcd. for C21H28N2O3: C, 70.76; H, 7.92; N, 7.86; Found: C, 70.81; 1H, 7.79; N, 7.70.

出典