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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
ノート
印刷プレビュー

反応式

HRID 873959 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 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

生成物 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
収率 68.5%

試薬・触媒・溶媒 5

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a0625580ca944c94ab065e33eee4b086
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08975417B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート