반응 #51740
ord-6a1054619fbc4fcb904c96e147584521
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1세척The organic layer was washed with 2N HCl, H2O, saturated sodium bicarbonate solution and brine
- 2건조was dried (MgSO4)
- 3기타The solvents were evaporated
- 4기타the residue was purified by flash chromatography (100% hexanes to 25% EtOAc in hexanes)
실험 절차
To 4-isopropyl-7-methyl-6-thiocyanato-benzothiazol-2-yl-amine (Example L-4; 4.0 g, 17 mmol) dissolved in CH2Cl2 (25 mL) and pyridine (5 mL), was added methyl chloroformate at 0° C. The reaction mixture was stirred at room temperature for 2 hours. H2O was added to the reaction mixture followed by EtOAc (100 mL). The organic layer was washed with 2N HCl, H2O, saturated sodium bicarbonate solution and brine, and was dried (MgSO4). The solvents were evaporated, and the residue was purified by flash chromatography (100% hexanes to 25% EtOAc in hexanes) to give 2-(methyloxycarbonyl)amino-4-isopropyl-7-methyl-6-thiocyanato-benzothiazole. MS (APCI): 322 (M+H).