HCID 10563902, compound → HCID 9992351, compound
Reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[S:8]([NH:11][C:12]([CH:14]1[CH2:18][CH2:17][CH2:16][CH2:15]1)=O)(=[O:10])=[O:9]>CN(C=O)C.P(Cl)(Cl)(Cl)=O>[CH:14]1([C:12]2[NH:1][C:2]3[CH:7]=[CH:6][N:5]=[CH:4][C:3]=3[S:8](=[O:10])(=[O:9])[N:11]=2)[CH2:18][CH2:17][CH2:16][CH2:15]1Participants
4
Reactant 1
Product 1
Reagents, catalysts & solvents 2
Procedure
A solution of 1 g of 4-amino-3-cyclopentylcarbonylaminosulfonylpyridine (Preparation 17) in 1 cm3 of DMF and 10 cm3 of phosphorus oxychloride is stirred at ambient temperature for 3 hours. The solvents are removed under partial vacuum (rotary evaporator) and the residue is dissolved in 10 cm3 of water. The solution is adjusted to a pH of 4 (NaHCO3) and the crystalline precipitate obtained is collected on a filter, washed with water and dried.
Workup
- customThe solvents are removed under partial vacuum (rotary evaporator)
- dissolutionthe residue is dissolved in 10 cm3 of water
- customthe crystalline precipitate obtained
- customis collected on a filter
- washwashed with water
- customdried
Sources & evidence
- ORD record
- ord-0e3365d861e146e4afc61a5e07c584dc
- Source dataset
- uspto-grants-1995_10
- Patent number
- US05459138
Reaction notes
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