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Cesium carbonate → HCID 42629845, 화합물

HRID 1880616
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HRID 1880616 반응식
Br.[Cl:2][C:3]1[C:12]([OH:13])=[C:11]([OH:14])[C:10]([Cl:15])=[C:9]2[C:4]=1[CH2:5][CH2:6][NH:7][CH2:8]2.[CH3:16][C:17]1[C:22](/[CH:23]=[CH:24]/[C:25](O)=[O:26])=[CH:21][CH:20]=[C:19]([C:28]([F:31])([F:30])[F:29])[N:18]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C1C=CN=CC=1)C.CN(C=O)C.O>[Cl:2][C:3]1[C:12]([OH:13])=[C:11]([OH:14])[C:10]([Cl:15])=[C:9]2[C:4]=1[CH2:5][CH2:6][N:7]([C:25](=[O:26])/[CH:24]=[CH:23]/[C:22]1[C:17]([CH3:16])=[N:18][C:19]([C:28]([F:29])([F:30])[F:31])=[CH:20][CH:21]=1)[CH2:8]2
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참가 물질

9

반응물 5

HCID 10796Cesium carbonateHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 57808084HCID 57808084, 화합물HCID 685081725,8-Dichloro-1,2,3,4-tetrahydroisoquinoline-6,7-diol hydrobromide

생성물 1

HCID 42629845
HCID 42629845, 화합물
수율 11%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

5,8-Dichloro-1,2,3,4-tetrahydroisoquinoline-6,7-diol hydro bromide (183 mg, 0.58 mmol), (E)-3-(2-methyl-6-(trifluoromethyl)pyridin-3-yl)acrylic acid (140 mg, 0.64 mmol), EDC.HCl (167 mg, 0.87 mmol), HOBt (89 mg, 0.58 mmol), DMAP (147 mg, 1.2 mmol) and Cs2CO3 (391 mg, 1.2 mmol) were suspended in DMF (15 mL) and stirred at rt for 12 h. The reaction mixture was then diluted with water (30 mL) and extracted with EtOAc (3×30 mL). Combined organics were washed with NaHCO3 (2×30 mL, sat. aq.), water (3×30 mL) and brine and dried (MgSO4). After filtration and evaporation the residue was purified by column chromatography (SiO2, CH2Cl2:MeOH 95:5) and was then further purified by size exclusion chromatography (sephadex, CHCl3:MeOH 1:1) to give the title compound (28 mg, 63 μmol, 11%) as a yellow solid.

후처리

  1. extractionextracted with EtOAc (3×30 mL)
  2. washCombined organics were washed with NaHCO3 (2×30 mL, sat. aq.), water (3×30 mL) and brine
  3. dry with materialdried (MgSO4)
  4. filtrationAfter filtration and evaporation the residue
  5. customwas purified by column chromatography (SiO2, CH2Cl2:MeOH 95:5)
  6. customwas then further purified by size exclusion chromatography (sephadex, CHCl3:MeOH 1:1)

출처 및 근거

ORD 기록
ord-8055999995444c849488fc6fc6192328
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318768B2

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