反应详情

温度

50 °C

A 0.5 M solution of zinc chloride in tetrahydrofuran (18.00 mL) is added dropwise at room temperature to a mixture of N-hydroxy-benzamidine (817 mg) and 1,4-dioxa-8-aza-spiro[4.5]decane-8-carbonitrile (1.00 g) in ethyl acetate (20 mL). The reaction mixture is stirred at 50° C. for 3 h and cooled to room temperature. The precipitate is filtered off and heated to 100° C. for 1 h in a mixture of ethanol (10 mL) and glacial acetic acid (5 mL). The solvents are evaporated and the crude product is purified by HPLC. TLC: rf=0.88 (silica gel, CH2Cl2/MeOH 9:1); Mass spectrum (ESI+): m/z=288 [M+H]+.

1. temperaturecooled to room temperature
2. filtrationThe precipitate is filtered off
3. temperatureheated to 100° C. for 1 h in a mixture of ethanol (10 mL) and glacial acetic acid (5 mL)
4. customThe solvents are evaporated
5. customthe crude product is purified by HPLC