반응 #684958

ord-b9add24f19a340a0a032660f8b46dec8

반응 방정식

O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
COC(C)(C)OC
2,2-Dimethoxypropane
CC1(C)C2CCC1(CS(=O)(=O)O)C(=O)C2
10-camphorsulfonic acid
CN(C)C=O
dimethylformamide
CC1(C)OCC(C#Cc2ccc(Cc3nccc4ccccc34)cc2)O1
title compound
CC1(C)OCC(C#Cc2ccc(Cc3nccc4ccccc34)cc2)O1
1-{4-[2-(2,2-Dimethyl-1,3-dioxolan-4-yl)-1-ethynyl]benzyl}-isoquinoline

반응 조건

온도
75°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the reaction mixture was extracted with ethyl acetate
  2. 2
    세척washed with water
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    농축concentrated under reduced pressure
  5. 5
    기타The residue was purified by silica gel column chromatography

실험 절차

2,2-Dimethoxypropane (0.36 ml), 10-camphorsulfonic acid (43 mg), and molecular sieves (4 Å) were added to a solution of the compound of Example B109 (34 mg) in dimethylformamide (2 ml), and this reaction mixture was stirred at 75° C. for 9 hours. After an saturated aqueous sodium carbonate solution was added, the reaction mixture was extracted with ethyl acetate, washed with water, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (14 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07897387B2uspto-grants-2011_03