Triethylamine → 2-Ethoxycarbonylaminomethyl-pyrimidine
Reaction equation
C(N(CC)CC)C.[NH2:8][CH2:9][C:10]1[N:15]=[CH:14][CH:13]=[CH:12][N:11]=1.[CH2:16]([O:18][C:19](Cl)=[O:20])[CH3:17]>C1(C)C=CC=CC=1>[CH2:16]([O:18][C:19]([NH:8][CH2:9][C:10]1[N:15]=[CH:14][CH:13]=[CH:12][N:11]=1)=[O:20])[CH3:17]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
49.5 g (0.49 mol) of triethylamine are added to 49.5 g (0.45 mol) of 2-aminomethyl-pyrimidine in 450 ml of toluene and then 52 g (0.48 mol) of ethyl chlorocarbonic acid are added dropwise under cooling with ice. The mixture is subsequently stirred at room temperature for 2 hours. Triethylamine hydrochloride is filtered off with suction, the filtrate is washed with brine, dried with MgSO4, concentrated, and distilled.
Workup
- temperatureunder cooling with ice
- filtrationTriethylamine hydrochloride is filtered off with suction
- washthe filtrate is washed with brine
- dry with materialdried with MgSO4
- concentrationconcentrated
- distillationdistilled
Sources & evidence
- ORD record
- ord-5b87c8e40bf3472fa51922030f5f156a
- Source dataset
- uspto-grants-1994_05
- Patent number
- US05312823
Reaction notes
Loading…