Hydrochloric Acid → HCID 20525070, compound
Reaction equation
[ClH:1].C(OC([NH:9][CH2:10][CH2:11][CH2:12][NH:13][C:14]([N:16]1[CH:23]=[C:22]([F:24])[C:20](=[O:21])[NH:19][C:17]1=[O:18])=[O:15])=O)(C)(C)C>C(O)C>[ClH:1].[NH2:9][CH2:10][CH2:11][CH2:12][NH:13][C:14]([N:16]1[CH:23]=[C:22]([F:24])[C:20](=[O:21])[NH:19][C:17]1=[O:18])=[O:15]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Hydrogen chloride gas was introduced to the solution of 1-[N-[3-(t-butoxycarbonylamino)propyl]carbamoyl]-5-fluorouracil (5.1 g.) which was prepared in Example 20 in ethanol (30 ml.) until precipitates were appeared for 1 hour with stirring under cooling with ice. The reaction mixture was further stirred for 1 hour at ambient temperature, and diethyl ether (100 ml.) was added therein. The resultant crystalline precipitates were collected by filtration and were dried over phosphoric anhydride to give 1-[N-(3-aminopropyl)carbamoyl]-5-fluorouracil hydrochloride (1.5 g.).
Workup
- customuntil precipitates
- temperatureunder cooling with ice
- stirringThe reaction mixture was further stirred for 1 hour at ambient temperature
- additiondiethyl ether (100 ml.) was added
- customThe resultant crystalline precipitates
- filtrationwere collected by filtration
- dry with materialwere dried over phosphoric anhydride
Sources & evidence
- ORD record
- ord-7d3ced70ccde4ad9858aa0392fd45052
- Source dataset
- uspto-grants-1982_09
- Patent number
- US04349552
Reaction notes
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