Triethylamine → HCID 11047717, compound

Participants

Reaction Steps

2HCl (2.93 g) was reacted with triethylamine (2.90 g) in ether (150 ml). The reaction mixture was filtered, and β-bromoethyl isocyanate (1.23 g) was added to the filtrate to give a white solid (3.32 g; melting point 103°-105° C.). The infrared absorption spectrum of the solid was as shown in FIG. 2. It was very similar to the infrared absorption spectrum of N-[p-bis(β-chloroethyl)aminophenyl]-N'-(β'-chloroethyl)urea obtained in Example 1, and showed a strong absorption based on the NH linkage at 3300 cm-1 and a strong absorption based on the carbonyl linkage of the ureido group at 1625 cm-1. The elemental analysis values were C 33.44%, H 3.47%, and N 8.84% which agreed with the calculated values for the composition formula C13H18N3OBr3 (472.04) which were C 33.908%, H 3.84%, N 8.90%. Its mass spectrum showed M⊕ at m/e=472 and peaks corresponding to [M⊕ -Br] at m/e=393 and 392. The foregoing results clearly show that the resulting white solid is N-[p-bis(β-bromoethyl)aminophenyl]-N'-(β'-bromoethyl)urea (designated as compound No. 1). The yield was 95.0%. ##STR13##

Provenance & Evidence