Water → HCID 178454308, compound
Reaction equation
O.[C:2]([NH:9][C:10]([NH:12]C(OC(C)(C)C)=O)=[NH:11])([O:4][C:5]([CH3:8])([CH3:7])[CH3:6])=[O:3]>CC(OC)(C)C>[C:5]([O:4][C:2]([NH:9][C:10]([NH2:12])=[NH:11])=[O:3])([CH3:8])([CH3:6])[CH3:7]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 57.5 °C
Procedure
After addition of water (200.00 g) the resultant mixture was evaporated to yield a solid comprising the crude product together with inorganic salts and a small amount of bis-Boc-guanidine. The solids were suspended in 2-Me-THF (344.00 g), the suspension was stirred and heated to reflux and maintained at reflux for about 1 h. The suspension was then cooled to about 55-60° C. and filtered warm to remove the inorganic salts. Evaporation of the 2-MeTHF yielded a solid. This solid was re-suspended in MTBE (37.00 g) and the resultant suspension was stirred at ambient temperature for ˜1 h. The suspension was filtered, and the solid was washed with MTBE (18.5 g). The MTBE treatment was repeated again and the resultant product was air dried for several hours at ambient temperature. The product —N-(t-butyloxycarbonyl)-guanidine—was isolated as a solid.
Workup
- customwas evaporated
- customto yield a solid comprising the crude product together with inorganic salts
- temperatureheated
- temperatureto reflux
- temperaturemaintained
- temperatureat reflux for about 1 h
- filtrationfiltered
- temperaturewarm
- customto remove the inorganic salts
- customEvaporation of the 2-MeTHF
- customyielded a solid
- filtrationThe suspension was filtered
- washthe solid was washed with MTBE (18.5 g)
- customdried for several hours at ambient temperature
Sources & evidence
- ORD record
- ord-031bf07535b94a7c91a7c91b898c343d
- Source dataset
- uspto-grants-2015_04
- Patent number
- US09006432B2
Reaction notes
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