Hydrochloric Acid → HCID 19973183, compound
Reaction equation
CC([N:5]([CH2:9][C:10](=[O:17])[NH:11][N:12]1[CH:16]=[CH:15][CH:14]=[CH:13]1)C(=O)[O-])(C)C.[ClH:18]>>[ClH:18].[NH2:5][CH2:9][C:10]([NH:11][N:12]1[CH:16]=[CH:15][CH:14]=[CH:13]1)=[O:17]Participants
3
Procedure
To 1,1-dimethylethyl-[2-oxo-2-(1H-pyrrol-1-ylamino)ethyl]carbamate (5.67 g) was added 35 ml of a 3.7M ethereal hydrogen chloride solution. The reaction mixture was stirred at room temperature over a period of 5 hours. The colored powder obtained by suction filtration was purified by addition of a solution of the product in methanol/diethyl ether, collecting the precipitate and repeating this procedure several times until the greater part of the substance was dissolved in the mother liquors. The last precipitate was discarded and the combined mother liquors were again recrystallized from methanol/diethyl ether. This afforded 1.90 g (46%) of the product as a powder, m.p. 212°-215° C. (dec.).
Workup
- customThe colored powder obtained by suction filtration
- customwas purified by addition of a solution of the product in methanol/diethyl ether
- customcollecting the precipitate
- dissolutionwas dissolved in the mother liquors
- customthe combined mother liquors were again recrystallized from methanol/diethyl ether
Sources & evidence
- ORD record
- ord-9abdea21c0c94ac4b94d2a2bd7f6ac22
- Source dataset
- uspto-grants-1995_06
- Patent number
- US05428053
Reaction notes
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