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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Cesium carbonate → 4-(4-chlorophenyl)-1-cyclopropyl-3-methyl-5-(3-methyl-3H-[1,2,3]triazolo[4,5-b]-pyridin-5-yl)-4,5-dihydropyrrolo[3,4-c]pyrazol-6(1H)-one

HRID 873959
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HRID 873959 반응식
Cl[C:2]1[N:7]=[C:6]2[N:8]([CH3:11])[N:9]=[N:10][C:5]2=[CH:4][CH:3]=1.[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([CH:19]2[C:26]3[C:25]([CH3:27])=[N:24][N:23]([CH:28]4[CH2:30][CH2:29]4)[C:22]=3[C:21](=[O:31])[NH:20]2)=[CH:15][CH:14]=1.CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.CCOC(C)=O.O.CCOCC.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([CH:19]2[C:26]3[C:25]([CH3:27])=[N:24][N:23]([CH:28]4[CH2:30][CH2:29]4)[C:22]=3[C:21](=[O:31])[N:20]2[C:2]2[N:7]=[C:6]3[N:8]([CH3:11])[N:9]=[N:10][C:5]3=[CH:4][CH:3]=2)=[CH:15][CH:14]=1
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참가 물질

10

반응물 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 846532705-Chloro-3-methyl-3H-[1,2,3]triazolo[4,5-B]pyridineHCID 1177027334-(4-chlorophenyl)-1-cyclopropyl-3-methyl-4,5-dihydropyrrolo[3,4-c]pyrazol-6(1H)-one

생성물 1

HCID 86293161
4-(4-chlorophenyl)-1-cyclopropyl-3-methyl-5-(3-methyl-3H-[1,2,3]triazolo[4,5-b]-pyridin-5-yl)-4,5-dihydropyrrolo[3,4-c]pyrazol-6(1H)-one
수율 68.5%

시약·촉매·용매 5

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 962Water용매HCID 3283Diethyl Ether용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A flask was charged with 5-chloro-3-methyl-3H-[1,2,3]triazolo[4,5-b]pyridine (Step 102.3) (132 mg, 0.782 mmol), 4-(4-chlorophenyl)-1-cyclopropyl-3-methyl-4,5-dihydropyrrolo[3,4-c]pyrazol-6(1H)-one (Step 85.6) (150 mg, 0.521 mmol) Pd2(dba)3 (47.7 mg, 0.052 mmol), Xantphos (60.3 mg, 0.104 mmol) and Cs2CO3 (340 mg, 1.043 mmol) in dioxane (3 mL) and the resulting mixture was heated up and stirred at 100° C. for 16 hr. The reaction was diluted with EtOAc and water and both phases separated. The aqueous layer was extracted with EtOAc, the combined organic layers were washed with water and brine, dried over Na2SO4 and concentrated under reduced pressure. Palladium was removed using a Varian PL-Thiol MP SPE cartridge and the residue was purified by silica gel column chromatography (50% EtOAc/hexane) to afford, after trituration in Et2O, the title product (153 mg, 0.357 mmol, 68% yield) as white solid. tR: 1.20 min (LC-MS 2); ESI-MS: 420 [M+H]+ (LC-MS 2); Rf=0.24 (50% EtOAc/Hexane); 1H NMR (400 MHz, DMSO-d6) δ ppm 0.99-1.16 (m, 2H) 1.21-1.35 (m, 2H) 1.95 (d, J=3.6 Hz, 3H) 3.87 (td, J=7.3, 3.6 Hz, 1H) 4.14 (d, J=3.7 Hz, 3H) 6.63 (d, J=3.6 Hz, 1H) 7.26-7.42 (m, 2H) 7.42-7.58 (m, 2H) 8.30-8.48 (m, 1H) 8.54 (dt, J=9.2, 3.2 Hz, 1H).

후처리

  1. temperaturethe resulting mixture was heated up
  2. customboth phases separated
  3. extractionThe aqueous layer was extracted with EtOAc
  4. washthe combined organic layers were washed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. customPalladium was removed
  8. customthe residue was purified by silica gel column chromatography (50% EtOAc/hexane)
  9. customto afford

출처 및 근거

ORD 기록
ord-a0625580ca944c94ab065e33eee4b086
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08975417B2

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