反応 #84149

反応方程式

4-nitro-1H-pyrazole

K2CO3

3-bromo-propanol

→

title compound

収率 93.0%

3-(4-Nitro-pyrazol-1-yl)-propan-1-ol

収率 93.0%

溶媒

MeCN

反応条件

後処理

1. 1
   その他The solvent was evaporated in vacuo
2. 2
   その他the residue partitioned between H2O (15 mL) and EtOAc (15 mL)
3. 3
   その他The layers were separated
4. 4
   抽出the aqueous phase extracted with EtOAc (2×15 mL)
5. 5
   乾燥The combined organics were dried (MgSO4)
6. 6
   ろ過filtered
7. 7
   その他the solvent evaporated in vacuo

実験手順

To a stirred solution of 4-nitro-1H-pyrazole (27) (1.0 g, 8.9 mmol) in MeCN (15 mL) was added K2CO3 (1.8 g, 13.2 mmol) and 3-bromo-propanol (880 μL, 9.7 mmol). The mixture was stirred at 75° C. for 6 hours. The solvent was evaporated in vacuo and the residue partitioned between H2O (15 mL) and EtOAc (15 mL). The layers were separated and the aqueous phase extracted with EtOAc (2×15 mL). The combined organics were dried (MgSO4), filtered and the solvent evaporated in vacuo to afford the title compound as a pale yellow oil (1.41 g, 93%); LCMS, Rt=1.31 min (MeOH-FA method), m/z 172 (MH+).

出典