Methane → HCID 53917812, compound
Reaction equation
[NH2:1][C:2]1[C:7]([S:8]([NH:11][C:12](=O)[CH3:13])(=[O:10])=[O:9])=[CH:6][N:5]=[C:4]([Cl:15])[CH:3]=1.C>C([O-])(O)=O.[Na+]>[Cl:15][C:4]1[N:5]=[CH:6][C:7]2[S:8](=[O:10])(=[O:9])[N:11]=[C:12]([CH3:13])[NH:1][C:2]=2[CH:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
0.2 g of 4-amino-5-acetylaminosulfonyl-2- chloropyridine (Preparation 19) is introduced into an open round-bottomed flask placed on an oil bath at 240° C. The temperature of the oil bath is brought over a period of a half-hour from 240° C. to 270° C. The molten mass is then cooled. It is dissolved in 4 cm3 of a tepid NaHCO3 solution (2% m/v). The solution is decolored with absorbing charcoal, filtered and then adjusted to a pH of 4 using formic acid. The crystalline precipitate obtained is collected on a filter, washed with water and dried.
Workup
- customplaced on an oil bath at 240° C
- waitThe temperature of the oil bath is brought over a period of a half-hour from 240° C. to 270° C
- temperatureThe molten mass is then cooled
- filtrationfiltered
- customThe crystalline precipitate obtained
- customis collected on a filter
- washwashed with water
- customdried
Sources & evidence
- ORD record
- ord-1994bc7f46bd4377bdf94a2097e5613a
- Source dataset
- uspto-grants-1995_10
- Patent number
- US05459138
Reaction notes
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