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Sodium Bicarbonate → HCID 67338716, 화합물

HRID 2092317
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HRID 2092317 반응식
I[C:2]1[C:11]([CH3:12])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][N:6]=[C:7]2[NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=1.[CH3:24][N:25]1[C:30]2[N:31]=[C:32]([NH:35][CH3:36])[N:33]=[CH:34][C:29]=2[CH:28]=[C:27](B2OC(C)(C)C(C)(C)O2)[C:26]1=[O:46].O.C(=O)([O-])[O-].[Na+].[Na+].C(=O)(O)[O-].[Na+]>CCOC(C)=O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O.CN(C=O)C>[CH3:24][N:25]1[C:30]2[N:31]=[C:32]([NH:35][CH3:36])[N:33]=[CH:34][C:29]=2[CH:28]=[C:27]([C:2]2[C:11]([CH3:12])=[CH:10][CH:9]=[C:8]3[C:3]=2[CH:4]=[CH:5][N:6]=[C:7]3[NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=2)[C:26]1=[O:46]
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참가 물질

9

반응물 4

HCID 516892Sodium BicarbonateHCID 2735133Sodium Carbonate MonohydrateHCID 58466448HCID 58466448, 화합물HCID 673385755-iodo-6-methyl-N-(3-(trifluoromethyl)phenyl)isoquinolin-1-amine

생성물 1

HCID 67338716HCID 67338716, 화합물수율 19.8%

시약·촉매·용매 4

HCID 178418476
HCID 178418476, 화합물
촉매
HCID 962Water용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

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온도
160 °C

실험 절차

To a solution of 5-iodo-6-methyl-N-(3-(trifluoromethyl)phenyl)isoquinolin-1-amine (0.1680 g, 0.392 mmol) in 10:1 DMF:Water (1.5 ml), charged to a 5 mL mircowave reaction vessel, 8-methyl-2-(methylamino)-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrido[2,3-d]pyrimidin-7(8H)-one (0.149 g, 0.471 mmol), dichlorobis(triphenyl-phosphine)palladium (ii) (0.0110 g, 0.0157 mmol), and sodium carbonate hydrate (0.102 g, 0.824 mmol) were added. The reaction mixture was stirred at 160° C. for 20 min. The reaction mixture was diluted with EtOAc and partioned with saturated sodium bicarbonate. The aqueous layer was extracted twice with EtOAc. The combined organics were washed with brine, dried over magnesium sulfate and concentrated under vacuum. The resulting residue was loaded on to silica and purified by silica gel chromatgraphy (ISCO 2×12.0 g, 0-6% MeOH in DCM, 45 min.) and HPLC to give 8-methyl-6-(6-methyl-1-(3-(trifluoromethyl)phenylamino)isoquinolin-5-yl)-2-(methylamino)pyrido[2,3-d]pyrimidin-7(8H)-one (.0381 g, 19.8% yield). MS (M+H)+ 491.

후처리

  1. additionwere added
  2. extractionThe aqueous layer was extracted twice with EtOAc
  3. washThe combined organics were washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under vacuum
  6. custompurified by silica gel chromatgraphy (ISCO 2×12.0 g, 0-6% MeOH in DCM, 45 min.) and HPLC

출처 및 근거

ORD 기록
ord-7b575bd03a194c609d95c3fe25b0bb1f
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08440674B2

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