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bis(3-methylsulfonyl-4-i-propylbenzoyl)guanidine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With potassium carbonate; sodium chloride; In hydrogenchloride; diethyl ether; water; N,N-dimethyl-formamide;
b Bis(3-methylsulfonyl-4-i-propylbenzoyl)guanidine The acid chloride 1 a) and 3.9 g of <strong>[159138-80-4]3-methylsulfonyl-4-i-propylbenzoylguanidine</strong> are dissolved in 50 ml of DMF, and 3.4 g of K2CO3 are then added. The mixture is stirred at RT for 4 h and then left to stand overnight. The solution is subsequently concentrated and the residue stirred up in 200 ml of water. The solid is filtered off and washed with 100 ml of water. This solid is then dissolved in 100 ml of EA and washed 1* with 10 ml of 1N HCl and then 1* with 50 ml of NaCl solution. Drying takes place over Na2SO4 and the solvent is removed in vacuo. A yellow solid is obtained which is purified by being triturated twice with 20 ml of diethyl ether and subsequently being filtered off. The product is dried in vacuo and 1.9 g are obtained of a white solid, mp 218-221 C. Rf (CH2Cl2/MeOH 20:1)=0.57 MS (ES): 508 (M+1).
With sodium hydroxide; In tetrahydrofuran; water; at 30 - 40℃; for 4.0h;
d) 4-lsopropyl-3-methylsulfonylbenzoylguanidine methanesulfonate from c) by reaction with thionyl chloride in toluene (reflux) for 1 hour. After evaporating the solvent, the residue is dissolved in THF and the solution is added to a mixture of guanidine hydrochloride, 2N NaOH and THF. After 4 hours at 30-40 C, the THF is removed by distillation and the crystalline 4-isopropyl-3- methylsulfonylbenzoylguanidine (m. p.: 226-228 C) is filtered off. Reaction with methanesulfonic acid follows to form the salt
(4-isopropyl-3-methanesulfonylbenzoyl)guanidine methanesulfonate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
d) 4-lsopropyl-3-methylsulfonylbenzoylguanidine methanesulfonate from c) by reaction with thionyl chloride in toluene (reflux) for 1 hour. After evaporating the solvent, the residue is dissolved in THF and the solution is added to a mixture of guanidine hydrochloride, 2N NaOH and THF. After 4 hours at 30-40 C, the THF is removed by distillation and the crystalline 4-isopropyl-3- methylsulfonylbenzoylguanidine (m. p.: 226-228 C) is filtered off. Reaction with methanesulfonic acid follows to form the salt
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