반응 #73939
ord-778d7f5e63f94085bc1bae2701c3a430
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1세척washed with NaHCO3 (50 mL)
- 2추출The aqueous layer was extracted with DCM (2×50 mL)
- 3세척the combined organic fractions washed with water (200 mL), brine (200 mL)
- 4건조dried over Na2SO4
- 5기타Removing the solvent
실험 절차
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.