Isopropylamine → HCID 10632459, compound
Reaction equation
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[S:8]([NH2:11])(=[O:10])=[O:9].[CH:12]([NH2:15])([CH3:14])[CH3:13]>CO>[CH:12]([NH:15][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[S:8]([NH2:11])(=[O:10])=[O:9])([CH3:14])[CH3:13]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
10 g of 4-chloropyridine-3-sulfonamide are dissolved in 50 cm3 of methanol and 50 cm3 of isopropylamine. The solution is introduced into a sealed tube and brought to 120° C. for 18 hours. After cooling, the reaction mixture is concentrated to dryness under vacuum (rotary evaporator) and the residue is taken up in 200 cm3 of water. The precipitate corresponding to the title compound is collected on a filter and washed with water. The precipitate is redissolved in 100 cm3 of dilute NaOH. The solution is decolored with charcoal, filtered and then acidified to a pH of 6.5-7. The crystalline precipitate obtained is collected on a filter, washed with water and dried.
Workup
- additionThe solution is introduced into a sealed tube
- temperatureAfter cooling
- concentrationthe reaction mixture is concentrated to dryness under vacuum (rotary evaporator)
- customThe precipitate corresponding to the title compound is collected on
- filtrationa filter
- washwashed with water
- dissolutionThe precipitate is redissolved in 100 cm3 of dilute NaOH
- filtrationfiltered
- customThe crystalline precipitate obtained
- customis collected on a filter
- washwashed with water
- customdried
Sources & evidence
- ORD record
- ord-03077c71aeb0444c961291f34c0c064d
- Source dataset
- uspto-grants-1995_10
- Patent number
- US05459138
Reaction notes
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