تفاعل #73939

ord-778d7f5e63f94085bc1bae2701c3a430

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed with NaHCO3 (50 mL)
  2. 2
    استخلاصThe aqueous layer was extracted with DCM (2×50 mL)
  3. 3
    غسيلthe combined organic fractions washed with water (200 mL), brine (200 mL)
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    أخرىRemoving the solvent

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541448B2uspto-grants-2013_09