Sodium Bicarbonate → HCID 58947962、化合物
反応式
[NH2:1][C:2]1([CH2:8][S:9]([N:12]([CH3:14])[CH3:13])(=[O:11])=[O:10])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[C:15](=O)(O)[O-:16].[Na+]>ClCCl>[N:1]([C:2]1([CH2:8][S:9]([N:12]([CH3:14])[CH3:13])(=[O:11])=[O:10])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]1)=[C:15]=[O:16]参加物
4
反応条件
- 温度
- 0 °C
実験手順
A solution of amine hydrochloride 1200-D (520 mg) in 40 mL of dichloromethane was treated with 20 mL of aqueous saturated sodium bicarbonate solution and stirred vigorously for 10 min at 0° C. Stirring was stopped and layers were allowed to separate. Phosgene (10 mL of 20% solution in toluene) was added to the organic layer (lower layer) in one portion. The mixture was vigorously stirred immediately after addition for 10 min at 0° C. and further stirred at room temp for 3 h. The mixture was diluted with 100 mL of dichloromethane and layers were separated. The organic layer was washed with 50 mL of cold aqueous saturated sodium bicarbonate solution and dried over magnesium sulfate. The organic layer was filtered and diluted with 15 mL of toluene. The resulting solution was concentrated under reduced pressure and the product 1200-E was maintained as a 0.2M solution.