Reaktion #526822

Reaktionsgleichung

cyanobenzyl formate

1,4,7-triazaheptane

triethylamine

→

1,7-Bis(benzyloxycarbonyl)-1,4,7-triazaheptane

Lösungsmittel

dichloromethane

dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeevaporated to dryness in a vacuum
2. 2
   Waschenwashed with sodium bicarbonate solution
3. 3
   TrocknenThe ether solution is dried on sodium sulfate
4. 4
   Sonstigeevaporated to dryness in a vacuum
5. 5
   SonstigeThe residue is crystallized from a little ethanol
6. 6
   SonstigeThe title compound crystallizes into white needles

Vorschrift

4.87 g (47.2 mmol) of 1,4,7-triazaheptane as well as 5 ml of triethylamine are dissolved in 100 ml of dichloroethane. The solution of 15.22 g (94.4 mmol) of cyanobenzyl formate in 200 ml of dichloromethane is instilled in this solution within 3 hours. It is allowed to stir for 2 more days at room temperature, then evaporated to dryness in a vacuum, taken up in diethyl ether and washed with sodium bicarbonate solution. The ether solution is dried on sodium sulfate and evaporated to dryness in a vacuum. The residue is crystallized from a little ethanol. The title compound crystallizes into white needles. Yield: 11.46 g (65.7% of theory) Melting point: 73°-75° C. Elementary analysis: Cld: C 64.67 H 6.78 N 11.31 Fnd: C 64.82 H 6.64 N 11.28

Quelle