Hydrochloric Acid → HCID 178479494, compound
Reaction equation
[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:25]=[CH:24][C:17]([C:18]([NH:20][C:21]([NH2:23])=[NH:22])=[O:19])=[CH:16][C:15]=2[C:26]([F:29])([F:28])[F:27])[CH2:10][CH2:9]1)=[O:7].[ClH:30]>CO>[ClH:30].[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[CH:25]=[CH:24][C:17]([C:18]([NH:20][C:21]([NH2:23])=[NH:22])=[O:19])=[CH:16][C:15]=2[C:26]([F:28])([F:29])[F:27])[CH2:12][CH2:13]1)=[O:7]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 10 °C
Procedure
15.1 g of 4-[4-(2-pyrrolylcarbonyl)-1-piperazinyl]-3-trifluoromethylbenzoylguanidine is taken up in 151 mL of methanol and the resulting suspension is cooled to about 10° C. 16 mL of a saturated ethereal HCl solution are added to this suspension which is thus acidified to a pH of between 1 and 2. Stirring is continued, while cooling with ice, until crystallization is complete. The crystals are suction filtered, washed with cold methanol, and then with cold diethyl ether. Yield: 16.19 g; melting point: 223° C. (uncorrected).
Workup
- temperaturewhile cooling with ice, until crystallization
- filtrationfiltered
- washwashed with cold methanol
Sources & evidence
- ORD record
- ord-64e568efa6f146318bdc8004d2acc93e
- Source dataset
- uspto-grants-2004_05
- Patent number
- US06730678B2
Reaction notes
Loading…