반응 #73995

ord-95863c3662234acd84e8475d0627460a

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축was concentrated under vacuum
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in 100 mL of ethyl acetate
  3. 3
    세척was washed with 2×20 mL of water
  4. 4
    건조dried over anhydrous sodium sulfate
  5. 5
    농축concentrated under vacuum
  6. 6
    기타This resulted in 1.8 g (85%) of N-(2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethyl)-3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzenesulfonamide as yellow oil

실험 절차

To 2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethanamine (1.5 g, 6.87 mmol, 1.79 equiv) in DCM (20 mL) was added triethylamine (1.5 g, 14.82 mmol, 3.86 equiv) and 3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzene-1-sulfonyl chloride (1.5 g, 3.84 mmol, 1.00 equiv). The reaction was stirred overnight at room temperature at which time the resulting mixture was concentrated under vacuum. The residue was dissolved in 100 mL of ethyl acetate and then was washed with 2×20 mL of water, dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 1.8 g (85%) of N-(2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethyl)-3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzenesulfonamide as yellow oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541448B2uspto-grants-2013_09