反応 #67941

反応方程式

amides

4-Amino-2-methoxy-3-[(1-methyl-4-nitro-1H-pyrrole-2-carbonyl)-amino]-benzoic Acid Methyl Ester

→

15

収率 85.5%

4-Methoxy-2-(1-methyl-4-nitro-1H-pyrrol-2-yl)-3H-benzimidazole-5-carboxylic Acid Methyl Ester

収率 85.5%

溶媒

acetic acid

反応条件

後処理

1. 1
   その他Most of the solvent was evaporated
2. 2
   ろ過the precipitate was filtered
3. 3
   洗浄washed with Et2O
4. 4
   その他Drying under hv

実験手順

The aforementioned mixture of amides 14a/14b (500 mg, 1.43 mmol) was suspended in glacial acetic acid (8 mL) and heated to 90° C. for 7 h. Most of the solvent was evaporated, and the yellow residue was suspended in Et2O. After being vigorously stirred for 20 min, the precipitate was filtered and washed with Et2O. Drying under hv gave 404 mg (85%) of 15 as a beige solid. Data of 15: Rf 0.80 (hexane/EtOAc 1:5). 1H NMR (300 MHz, DMSOd6): δ 3.76 (s, 3H), 4.14 (s, 3H), 4.34 (s, 3H), 7.14-7.17 (m, 1H), 7.48-7.55 (m, 3H), 8.25 (s, 1H). MS (ESI): m/z (rel intensity) 331 (98).

出典