反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Pyridine (3.09 mL, 38.4 mmol) was added to a solution of 4-fluoroaniline (3.73 g, 33.6 mmol) in chloroform (107 mL), and 7-bromo-2-(trifluoroacetyl)-1,2,3,4-tetrahydroisoquinoline-6-sulfonyl chloride (13.0 g, 32.0 mmol) was added thereto while cooling in ice. The mixture was warmed to room temperature and stirred for 13 hr. To the mixture was added 1 mol/L hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was concentrated under reduced pressure and the concentrate was powdered with hexane and ethyl acetate (4:1) and then collected by filtration to afford 7-bromo-N-(4-fluorophenyl)-2-(trifluoroacetyl)-1,2,3,4-tetrahydroisoquinoline-6-sulfonamide as an orange powder (14.5 g).
WORKUP
后处理
- additionwas added
- temperaturewhile cooling in ice
- extractionthe mixture was extracted with chloroform
- concentrationThe organic layer was concentrated under reduced pressure
- filtrationcollected by filtration