1,3-Propanediamine → tert-Butyl (3-aminopropyl)carbamate
Reaction equation
C(O[C:6](=[O:12])[O:7][C:8]([CH3:11])([CH3:10])[CH3:9])(C)(C)C.[NH2:13][CH2:14][CH2:15][CH2:16][NH2:17]>C(Cl)Cl>[C:8]([O:7][C:6]([NH:13][CH2:14][CH2:15][CH2:16][NH2:17])=[O:12])([CH3:9])([CH3:10])[CH3:11]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 20 °C
Procedure
A solution of 46 g of di-tert-butyl-carbonate in 120 ml of methylene chloride was added at +5° C. without exceeding +10° C. to a solution of 36 ml of 1,3-diamino-propane in 160 ml of methylene chloride and after stirring for 16 hours at 20° C., the insoluble part was filtered off. The filtrate was evaporated to dryness under vacuum to obtain 63 g of residue which was chromatographed on silica (eluant: methanol with 2% ammonia) to obtain 23 g of the expected product melting at <60° C.
Workup
- filtrationthe insoluble part was filtered off
- customThe filtrate was evaporated to dryness under vacuum
Sources & evidence
- ORD record
- ord-ed69bd0f138d4d92aa22ac1a621f6ed5
- Source dataset
- uspto-grants-1991_11
- Patent number
- US05064861
Reaction notes
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