反応 #1687655

反応方程式

2,6-dihydroxyanthraquinone

diethyl(4-bromobutyl)phosphonate

K2CO3

→

2,6-Bis (4-phosphonobutyloxy)-anthraquinone

溶媒

DMF

反応条件

後処理

1. 1
   抽出The solution was extracted with CH2Cl2
2. 2
   乾燥The CH2Cl2 solution was dried
3. 3
   その他leaving a yellow solid
4. 4
   その他The ester was purified by column chromatography
5. 5
   workup.ADDITIONfollowed by addition of water
6. 6
   洗浄The bisphosphonic acid derivative was washed with CH2Cl2
7. 7
   ろ過filtered
8. 8
   その他collected

実験手順

2,6-dihydroxyanthraquinone (1.19 g, 4.98 mmol) and diethyl(4-bromobutyl)phosphonate (3.0 g, 10 mmol) were heated at 60 ° C. in 5 ml DMF in the presence of 0.8 g of K2CO3 for 72 hours. The solution was extracted with CH2Cl2. The CH2Cl2 solution was dried, leaving a yellow solid. The ester was purified by column chromatography. The bisphosphonate ester was converted to the acid by overnight stirring with 4-fold excess of bromotrimethylsilane in dry dichloromethane followed by addition of water. The bisphosphonic acid derivative was washed with CH2Cl2, filtered and collected.

出典