반응 #2175451

반응 방정식

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

HCl

→

9-hydroxymethyl-2,7-diaminofluorene dihydrochloride

용매

1,4-dioxane

반응 조건

후처리

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

실험 절차

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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