反応 #315031

反応方程式

morpholine

K3PO4

methyl 4-bromobenzoate

→

colorless solid

収率 80.5%

N-(4-Carbomethoxyphenyl)morpholine

収率 80.5%

溶媒

DME

反応条件

後処理

1. 1
   その他An oven-dried resealable Schlenk tube was purged with argon
2. 2
   その他The tube was purged with argon
3. 3
   その他fitted with a rubber septum
4. 4
   その他The septum was removed
5. 5
   その他the tube was sealed with a teflon
6. 6
   その他screw cap
7. 7
   温度The reaction mixture was then cooled to room temperature
8. 8
   workup.ADDITIONdiluted with EtOAc (20 mL)
9. 9
   ろ過filtered through celite and
10. 10
    濃縮concentrated in vacuo
11. 11
    その他The crude material was purified by flash chromatography on silica gel

実験手順

An oven-dried resealable Schlenk tube was purged with argon and charged with Pd2(dba)3 (2.3 mg, 0.0025 mmol, 1.0 mol % Pd), 2 [Example 1] (3.0 mg, 0.0076 mmol, 1.5 mol %), K3PO4 (150 mg, 0.71 mmol), and methyl 4-bromobenzoate (108 mg, 0.50 mmol). The tube was purged with argon, fitted with a rubber septum and then DME (1.0 mL) and morpholine (55 μL, 0.63 mmol) were added. The septum was removed, the tube was sealed with a teflon screw cap and the mixture was stirred at 80° C. for 24 h. The reaction mixture was then cooled to room temperature, diluted with EtOAc (20 mL), filtered through celite and concentrated in vacuo. The crude material was purified by flash chromatography on silica gel to afford 89 mg (80%) of a colorless solid.

出典