反応 #2175451

反応方程式

9-Hydroxymethyl-2,7-di(Boc-amino)fluorene

HCl

→

9-hydroxymethyl-2,7-diaminofluorene dihydrochloride

溶媒

1,4-dioxane

反応条件

後処理

1. 1
   その他The reaction solvents were removed at reduced pressure (45° C.)
2. 2
   workup.DISSOLUTIONThe product was dissolved in methanol
3. 3
   その他evaporated (2 times)
4. 4
   workup.DISSOLUTIONThe product was dissolved in methanol (8 mL)
5. 5
   その他precipitated by the slow addition of diethyl ether
6. 6
   温度cooling (repeat)

実験手順

9-Hydroxymethyl-2,7-di(Boc-amino)fluorene (0.39 g, 0.9 mmol) was dissolved in 1,4-dioxane. At 0° C. concentrated HCl (2.5 mL) was added and the reaction was stirred for two hours at 0° C. and for one hour at room temperature. The reaction solvents were removed at reduced pressure (45° C.). The product was dissolved in methanol and evaporated (2 times). The product was dissolved in methanol (8 mL) and precipitated by the slow addition of diethyl ether and cooling (repeat). The product was a red-orange solid (0.25 g, 91%) that showed a single spot by TLC (chloroform/methanol/acetic acid 85:15:3, ninhydrin stain). 1H-NMR (CD3OD): δ (ppm) 8.1 (d, 2H, Ar); 7.8 (s, 2H, Ar); 7.5 (d, 2H, Ar); 4.3 (t, 1H, CH); 4.0 (d, 2H, CH2)

出典