[CH:1]1([NH:4][CH2:5][CH:6]2[CH2:11][CH2:10][CH2:9][CH2:8][O:7]2)[CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl:19][C:20](Cl)([O:22]C(=O)OC(Cl)(Cl)Cl)Cl.O>C1COCC1.CN(C)C1C=CN=CC=1>[CH:1]1([N:4]([CH2:5][CH:6]2[CH2:11][CH2:10][CH2:9][CH2:8][O:7]2)[C:20]([Cl:19])=[O:22])[CH2:3][CH2:2]1To a stirred solution of cyclopropyl-(tetrahydro-pyran-2-ylmethyl)-amine (200 mg, 0.74 mmol) in THF (4 mL) is added triethylamine (144 μL, 1.036 mmol) and 4-dimethylaminopyridine (1.81 mg, 0.015 mmol). The mixture is cooled to 0° C., and triphosgene (88 mg, 0.296 mmol) is added in one portion. After stirring for 30 min at 0° C. and overnight at RT, water is cautiously added and the solution is extracted with AcOEt. The combined organic extracts are washed with brine, dried over Na2SO4, filtered and concentrated. TLC, Rf (CH2Cl2/MeOH 95:5)=0.9.
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