Reaktion #2175451

Reaktionsgleichung

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

HCl

→

9-hydroxymethyl-2,7-diaminofluorene dihydrochloride

Lösungsmittel

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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)

Quelle