反应详情

An ice-cooled solution of 302 mg (0.99 mmol) of the compound from Example 101A in 10 ml of dichloromethane was admixed dropwise with 99 μl (1.09 mmol) of 2-bromoethyl isocyanate. After 10 minutes, the ice bath was removed and the mixture was stirred for a further 5 min. All of the volatile components were removed on a rotary evaporator. The residue was taken up in 5 ml of anhydrous THF and admixed, with ice cooling, with 44 mg of sodium hydride (60% in mineral oil, 1.09 mmol). After 2 h, 1 ml of 1M hydrochloric acid was added and the reaction mixture was freed from the solvent on a rotary evaporator. The aqueous residue was dissolved in DMSO and purified by preparative HPLC [Method 23]. The product fraction was freed from the solvents on a rotary evaporator. Drying of the residue in an HV gave 210 mg (38% of theory) of the title compound.

1. customthe ice bath was removed
2. customAll of the volatile components were removed on a rotary evaporator
3. waitAfter 2 h
4. customthe reaction mixture was freed from the solvent on a rotary evaporator
5. dissolutionThe aqueous residue was dissolved in DMSO
6. custompurified by preparative HPLC [Method 23]
7. customThe product fraction was freed from the solvents on a rotary evaporator
8. customDrying of the residue in an HV