反应详情

2-(6-Cyclohexyl-3,4-dihydro-1H-isoquinoline-2-sulfonylmethyl)-3-methyl-butyric acid (143 mg) was dissolved in dichloromethane (15 ml) under a nitrogen atmosphere and oxalyl chloride (0.15 ml) added, followed by a solution of 10% N,N-dimethylformamide in dichloromethane (7 drops). The reaction was stirred at room temperature for 2 h then evaporated under reduced pressure and azeotroped with 1:1 dichloromethane-hexane (2×10 ml). The residue was dried under vacuum then suspended in tetrahydrofuran (15 ml) and treated with 50% wt solution of aqueous hydroxylamine (0.7 ml). The mixture was left to stir at room temperature for 1 h then evaporated under reduced pressure. The residue was triturated with water (20 ml) and the resulting solid filtered off, washed with water (10 ml) and dried under vacuum at 40° C. to give the title compound (120 mg, 82%).

1. customthen evaporated under reduced pressure
2. customazeotroped with 1:1 dichloromethane-hexane (2×10 ml)
3. customThe residue was dried under vacuum
4. additiontreated with 50% wt solution of aqueous hydroxylamine (0.7 ml)
5. waitThe mixture was left
6. stirringto stir at room temperature for 1 h
7. customthen evaporated under reduced pressure
8. customThe residue was triturated with water (20 ml)
9. filtrationthe resulting solid filtered off
10. washwashed with water (10 ml)
11. customdried under vacuum at 40° C.