反应 #69682

反应方程式

2-(2,4-dimethoxy-benzyl)-5-nitro-2,3-dihydro-1H-isoindole

anisole

TFA

→

5-nitro-2,3-dihydro-1H-isoindole trifluoroacetic acid salt

反应条件

后处理

1. 1
   其他The reaction mixture was evaporated in vacuo
2. 2
   其他the residue partitioned between DCM and water
3. 3
   其他The water layer was separated
4. 4
   洗涤washed with DCM (×3)
5. 5
   其他then evaporated
6. 6
   其他re-evaporated with toluene/MeOH (×3)

实验过程

2-(2,4-dimethoxy-benzyl)-5-nitro-2,3-dihydro-1H-isoindole (13 g) in TFA (18 ml) was treated with anisole (6 ml) then heated in a CEM microwave synthesiser at 120° C. (30 Watts) for 20 minutes (carried out batch wise, 6 times). The reaction mixture was evaporated in vacuo and the residue partitioned between DCM and water. The water layer was separated, washed with DCM (×3) then evaporated and re-evaporated with toluene/MeOH (×3) to give 9.8 g of 5-nitro-2,3-dihydro-1H-isoindole trifluoroacetic acid salt as a beige solid. 1H NMR (DMSO-d6) 9.85 (2H, br s), 8.32 (1H, d), 8.25 (1H, dd), 7.70 (1H, d), 4.68 (2H, s), 4.65 (2H, s).

来源