تفاعل #2175451

معادلة التفاعل

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

HCl

→

9-hydroxymethyl-2,7-diaminofluorene dihydrochloride

المذيبات

1,4-dioxane

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction solvents were removed at reduced pressure (45° C.)
2. 2
   workup.DISSOLUTIONThe product was dissolved in methanol
3. 3
   أخرىevaporated (2 times)
4. 4
   workup.DISSOLUTIONThe product was dissolved in methanol (8 mL)
5. 5
   أخرىprecipitated by the slow addition of diethyl ether
6. 6
   درجة الحرارةcooling (repeat)

الإجراء التجريبي

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)

المصدر