反応 #307272

反応方程式

5-amino-1-[6-(tert-butoxycarbonyl-methyl-amino)-pyrimidin-4-yl]-1H-pyrazole-4-carboxylic acid ethyl ester

lithium hydroxide

HCl

→

5-amino-1-[6-(tert-butoxycarbonyl-methyl-amino)-pyrimidin-4-yl]-1H-pyrazole-4-carboxylic acid

溶媒

1,4-Dioxane

water

反応条件

後処理

1. 1
   その他to form
2. 2
   ろ過After filtration
3. 3
   洗浄the undissolved solid is washed with small amount of water
4. 4
   その他air-dried

実験手順

A mixture of 5-amino-1-[6-(tert-butoxycarbonyl-methyl-amino)-pyrimidin-4-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (5.5 g, 15.2 mmol), lithium hydroxide (1.82 g, 75.8 mmol) dissolved in a mixture of 1,4-Dioxane (20 mL) and water (5 mL) is heated to 85° C. for 8 hours. The reaction mixture is then neutralized with 2 M HCl aqueous solution until pH˜4-5 causing a white precipitate to form. After filtration, the undissolved solid is washed with small amount of water, air-dried to give 5-amino-1-[6-(tert-butoxycarbonyl-methyl-amino)-pyrimidin-4-yl]-1H-pyrazole-4-carboxylic acid as white powder: 1H NMR 400 MHz (d6-DMSO) δ 8.41 (s, 1H), 8.00-7.40 (m, 4H), 6.86-6.58 (m, 1H), 2.86 (s, 3H); MS m/z 235.10 (M+1).

出典