反応 #51908

反応方程式

ethyl 7-hydroxy-2-(hydroxymethyl)-3-methylthieno[3,2-b]pyridine-6-carboxylate

4-fluorobenzylamine

→

title compound

収率 85.5%

N-(4-fluorobenzyl)-7-hydroxy-2-(hydroxymethyl)-3-methylthieno[3,2-b]pyridine-6-carboxamide

収率 85.5%

溶媒

HCl

反応条件

後処理

1. 1
   温度The mixture was then cooled to room temperature
2. 2
   温度cooled in the refrigerator for three hours
3. 3
   ろ過The resulting mixture was then filtered
4. 4
   洗浄the obtained solid was washed with 1N HCl several times (50 mL total volume)
5. 5
   その他dried in a vacuum oven at 60° C. over night

実験手順

A suspension of 140 mg (0.52 mmol) ethyl 7-hydroxy-2-(hydroxymethyl)-3-methylthieno[3,2-b]pyridine-6-carboxylate in 1.28 mL (11.2 mmol) 4-fluorobenzylamine was heated to 80° C. for 24 hours. The mixture was then cooled to room temperature and added to 10 mL of 1N HCl and then cooled in the refrigerator for three hours. The resulting mixture was then filtered and the obtained solid was washed with 1N HCl several times (50 mL total volume) and dried in a vacuum oven at 60° C. over night to provide 154 mg of the title compound as a tan solid.

出典