反应详情

Prepared as described in General Procedure 1. To methyl urea (0.24 g) in tetrahydrofuran was added sodium hydride (22 mg of 60% in oil) and the reaction mixture stirred for 50 min at room temp. Dicyclohexyl carbamoyl chloride (0.8 g) was then added (ice bath cooling used during addition) and the mixture was stirred overnight. The reaction mixture was then added to 0.5 ml water, partially concentrated in vacuo and water (2 mL) and ethyl acetate (10 mL) was added. The non soluble material was removed by filtration and the organic layer collected and concentrated in vacuo. An aliquot of the crude was then dissolved in THF and purified by preparative LCMS to give the desired product (8 mg).

1. customPrepared
2. temperature(ice bath cooling used during addition)
3. stirringthe mixture was stirred overnight
4. concentrationpartially concentrated in vacuo and water (2 mL) and ethyl acetate (10 mL)
5. additionwas added
6. customThe non soluble material was removed by filtration
7. customthe organic layer collected
8. concentrationconcentrated in vacuo
9. dissolutionAn aliquot of the crude was then dissolved in THF
10. custompurified by preparative LCMS