反应详情

To a solution of triphosgene (77 mg, 0.259 mmol) in CH2Cl2 (1 mL) at −78° C. is added dropwise pyridine (63 μl, 0.786 mmol) followed by a solution of cyclohexylmethyl-methylamine (100 mg, 0.786 mmol) in CH2Cl2 (1 mL). The yellow mixture is allowed to reach RT and stirred overnight. The solvent is concentrated, and the residue taken up in AcOEt. An aqueous saturated solution of NaHCO3 is added, the layers are separated and the aqueous one is extracted twice with AcOEt. The combined organic extracts are washed with brine, dried over Na2SO4, filtered and concentrated to afford the title compound as a yellow oil. TLC, Rf (CH2Cl2/MeOH 95:5)=0.95. MS (LC-MS): 189.1 [M+H]+.

1. customto reach RT
2. concentrationThe solvent is concentrated
3. additionAn aqueous saturated solution of NaHCO3 is added
4. customthe layers are separated
5. extractionthe aqueous one is extracted twice with AcOEt
6. washThe combined organic extracts are washed with brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated