Реакция #2175451

Уравнение реакции

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

HCl

→

9-hydroxymethyl-2,7-diaminofluorene dihydrochloride

Растворители

1,4-dioxane

Условия реакции

Обработка

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

Методика

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)

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