反应 #73939

ord-778d7f5e63f94085bc1bae2701c3a430

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with NaHCO3 (50 mL)
  2. 2
    萃取The aqueous layer was extracted with DCM (2×50 mL)
  3. 3
    洗涤the combined organic fractions washed with water (200 mL), brine (200 mL)
  4. 4
    干燥dried over Na2SO4
  5. 5
    其他Removing the solvent

实验过程

To a solution of 3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzene-1-sulfonyl chloride (intermediate 1.6) (600 mg, 1.41 mmol) in chloroform (2.82 mL) was added DIEA (545.7 mg, 4.24 mmol) and 2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethanamine (616.3 mg, 2.82 mmol). The reaction was stirred overnight at which point the mixture was diluted with 50 mL DCM and washed with NaHCO3 (50 mL). The aqueous layer was extracted with DCM (2×50 mL) and the combined organic fractions washed with water (200 mL), brine (200 mL), and dried over Na2SO4. Removing the solvent gave the title compound as an oil which was used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08541448B2uspto-grants-2013_09