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Sodium Carbonate → 4-bromo-1-methyl-3-(1-methylindolin-6-yl)-1H-pyrrolo[2,3-b]pyridine

HRID 330996
ノート
印刷プレビュー

反応式

HRID 330996 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[N:8]([CH3:12])[CH:9]=[C:10](I)[C:3]=12.[CH3:13][N:14]1[C:22]2[C:17](=[CH:18][CH:19]=[C:20](B3OC(C)(C)C(C)(C)O3)[CH:21]=2)[CH2:16][CH2:15]1.C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C.CN(C=O)C.C(Cl)Cl.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>[Br:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[N:8]([CH3:12])[CH:9]=[C:10]([C:20]3[CH:21]=[C:22]4[C:17]([CH2:16][CH2:15][N:14]4[CH3:13])=[CH:18][CH:19]=3)[C:3]=12
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

9

反応物 3

HCID 10340Sodium CarbonateHCID 709799671-Methyl-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)indolineHCID 710901484-bromo-3-iodo-1-methyl-1H-pyrrolo[2,3-b]pyridine

生成物 1

HCID 710903864-bromo-1-methyl-3-(1-methylindolin-6-yl)-1H-pyrrolo[2,3-b]pyridine収率 48.8%

試薬・触媒・溶媒 5

HCID 178418476
HCID 178418476、化合物
触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒
HCID 6342Acetonitrile溶媒
HCID 6344Dichloromethane溶媒2 回

反応条件

温度
55 °C

実験手順

To a stirred solution of 4-bromo-3-iodo-1-methyl-1H-pyrrolo[2,3-b]pyridine (D7) (5 g, 14.84 mmol) and 1-methyl-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)indoline (4.61 g, 17.81 mmol) in ACN (40 mL), DMF (40 mL) and DCM (20 mL) was added 2M sodium carbonate aq. solution (74.2 mL, 148 mmol). Bis(triphenylphosphine)palladium(II) chloride (1.250 g, 1.781 mmol) was then added to the solution and the resulting mixture was heated at 55° C. for ca. 1.5 hour. The reaction mixture was diluted with DCM (100 mL) and water (150 mL). The organic phase was separated and the aqueous phase was further extracted with DCM (100 mL×3). The combined organics were dried and concentrated. The residue was purified by chromatography on silica, eluting with a gradient of 0-20% ethyl acetate in cyclohexane. The corresponding fractions were combined and concentrated to give the title compound (2.48 g). LCMS (A): m/z (M+H)+ 342/344, C17H16BrN3 requires 341/343 (acidic).

後処理

  1. customThe organic phase was separated
  2. extractionthe aqueous phase was further extracted with DCM (100 mL×3)
  3. customThe combined organics were dried
  4. concentrationconcentrated
  5. customThe residue was purified by chromatography on silica
  6. washeluting with a gradient of 0-20% ethyl acetate in cyclohexane
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-b072d1a30e0442cf89e12e65e6d0669e
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877742B2

反応ノート

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