HCID 19012102, compound → HCID 21688812, compound
Reaction equation
[CH3:1][N:2]1[C:7]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([S:24][CH3:25])=[CH:20][C:19]=3[N+:26]([O-])=O)[CH2:10][CH2:9]2)=[CH:6][C:5](=[O:29])[N:4]([CH3:30])[C:3]1=[O:31]>C(O)C>[CH3:1][N:2]1[C:7]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([S:24][CH3:25])=[CH:20][C:19]=3[NH2:26])[CH2:10][CH2:9]2)=[CH:6][C:5](=[O:29])[N:4]([CH3:30])[C:3]1=[O:31]Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 70 °C
Procedure
2.0 g of the Compound v obtained in Reference Example 17 was dissolved in 20 ml of ethanol, and 4.5 g of stannic chloride (II) was added dropwise. The solution was heated up to 70° C. and then stirred for 30 minutes. The precipitated insolubles were removed by filtration, and the filtrate was then diluted with 100 ml of chloroform. Next, 20 ml of a 1N aqueous sodium hydroxide solution was added to the solution, followed by stirring vigorously. The formed insolubles were removed by filtration, and the resultant chloroform layer was separated, washed with water, dried over anhydrous sodium sulfate and then concentrated. The thus obtained oily product was purified through a silica gel column chromatograph (chloroform/methanol=100/1 in volume ratio), thereby obtaining 0.62 g of 1,3-dimethyl-6-[4-(3-[2-amino-4-methylmercaptophenoxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound 114).