克伦特罗杂质11

实验步骤: 11-18 15:58: 反应在N2保护下进行，往50ml干燥的双口瓶中，NCS（120mg,1.1eq）溶于0.5 mlACN中，将SM1(100ml,1eq)溶于0.5 mlACN中缓慢滴加入体系，室温搅拌3h LCMS或点板检测反应进程 后处理：减压蒸馏除去溶剂，加入水，用EA萃取，合并有机相用盐水洗涤，无水硫酸钠干燥，减压蒸馏浓缩得到粗品，粗品经TLC刮板会变坏

实验步骤: 11-18 15:53: 反应在N2保护下进行，往50ml干燥的双口瓶中，SM1（100mg,1eq）溶于0.5 mlACN中，将NCS(120ml,1.1eq)溶于0.5 mlACN中缓慢滴加入体系，室温搅拌过夜 LCMS或点板检测反应进程 后处理：减压蒸馏除去溶剂，加入水，用EA萃取，合并有机相用盐水洗涤，无水硫酸钠干燥，减压蒸馏浓缩得到粗品，粗品经TLC刮板会变坏

实验步骤: 11-23 11:33: 反应在N2保护下进行，往50ml干燥的双口瓶中，SM1（300mg,1eq）溶于3 mlACN中，将NCS(360ml,1.1eq)溶于3 mlACN中缓慢滴加入体系，室温搅拌过夜 LCMS或点板检测反应进程，直接用于下一步

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of sodium nitrite (1.63 g) in water (4.3 ml) was added dropwise to a solution of 4'-amino-3'-chloroacetophenone (2.5 g) and concentrated hydrochloric acid (5.5 ml) in water (5.5 ml) at 0° to 3° C., and the solution was stirred for 15 minutes at 0° C. The resulting solution was added portionwise to a mixture of sodium nitrite (7.3 g) and cuprous oxide (0.76 g) in water (32 ml) at -5° to 0° C. The mixture was stirred for 1 hour at 0° C. and for 1 hour at room temperature, and extracted with chloroform. The extract was washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel (60 g) eluting with chloroform. The fractions containing the desired compound were combined and concentrated under reduced pressure to give pale yellow crystals of 3'-chloro-4'-nitroacetophenone (2.2 g). The mixture was stirred for 1 hour at 0° C. and for 1 hour at room temperature extracted with chloroform The extract was washed with a saturated aqueous solution of sodium chloride dried over magnesium sulfate concentrated under reduced pressure eluting with chloroform The fractions containing the desired compound concentrated under reduced pressure

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of p-aminoacetophenone (20 g), pyridine (11.7 g), and iodobenzene dichloride (40 g) in tetrahydrofuran (300 ml) was stirred for 5 hours at 0° C. The insoluble materials were filtered, and the filtrate was concentrated under reduced pressure. The residue obtained was crystallized from ethanol to give colorless crystals of 4'-amino-3'-chloroacetophenone (20.1 g). The insoluble materials were filtered the filtrate was concentrated under reduced pressure The residue obtained was crystallized from ethanol