反応 #1583894

反応方程式

Sulfuric acid

7-methyl-2-propyl-3H-benzoimidazole-5-carboxylic acid

MeOH

→

Intermediate ( 7a )

収率 92.1%

7-Methyl-2-propyl-3H-benzoimidazole-5-carboxylic acid methyl ester

収率 92.1%

反応条件

後処理

1. 1
   温度The mixture was refluxed for 36 hours
2. 2
   濃縮concentrated in vacuo
3. 3
   workup.DISSOLUTIONThe recovered material was dissolved in 500 ml, EtOAc
4. 4
   洗浄washed with a saturated NaHCO3 solution
5. 5
   乾燥The organic layer was dried over MgSO4
6. 6
   濃縮concentrated

実験手順

Sulfuric acid (12 mL, 0.22 mol) was added to 7-methyl-2-propyl-3H-benzoimidazole-5-carboxylic acid (30 g, 136 mmol) dissolved in MeOH (670 mL, 16 mol). The mixture was refluxed for 36 hours and concentrated in vacuo. The recovered material was dissolved in 500 ml, EtOAc and washed with a saturated NaHCO3 solution. The organic layer was dried over MgSO4 and concentrated to provide Intermediate (7a) as a brown solid (29.1 g). MS m/z: [M+H+] calcd for C13H16N2O2, 233.1. found 233.2.

出典