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Potassium Carbonate → 6-chloro-5-[4-(1-methylpyrrolidin-3-yl)phenyl]-1H-indole-3-carbaldehyde

HRID 338402
ノート
印刷プレビュー

反応式

HRID 338402 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[CH:7][NH:8]2)=[CH:4][C:3]=1B1OCC(C)(C)CO1.[C:19](=[O:22])([O-])[O-].[K+].[K+].Br[C:26]1[CH:31]=[CH:30][C:29]([CH:32]2[CH2:36][CH2:35][N:34]([CH3:37])[CH2:33]2)=[CH:28][CH:27]=1>O1CCOCC1.CN(C=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([CH:19]=[O:22])=[CH:7][NH:8]2)=[CH:4][C:3]=1[C:26]1[CH:27]=[CH:28][C:29]([CH:32]2[CH2:36][CH2:35][N:34]([CH3:37])[CH2:33]2)=[CH:30][CH:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 594284273-(4-Bromophenyl)-1-methylpyrrolidineHCID 866987336-chloro-5-(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)-1H-indole

生成物 1

HCID 866987406-chloro-5-[4-(1-methylpyrrolidin-3-yl)phenyl]-1H-indole-3-carbaldehyde収率 152.2%

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 6228Dimethylformamide溶媒
HCID 312751,4-Dioxane溶媒

実験手順

To 6-chloro-5-(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)-1H-indole (118 mg, 0.446 mmol) in anhydrous 1,4-dioxane (3.7 mL) and anhydrous DMF (0.74 mL) was added N,N-dimethylformiminium chloride (114 mg, 0.892 mmol). The reaction mixture was stirred for 10 min at room temperature, yielding a thick suspension. The reaction mixture was treated with 2N aqueous potassium carbonate (1.1 mL, 2.2 mmol), 3-(4-bromophenyl)-1-methylpyrrolidine (120 mg, 0.446 mmol), and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (26 mg, 0.036 mmol). The resulting mixture was heated at 90° C. for 30 min. The reaction mixture was cooled and partitioned between water and EtOAc. The aqueous phase was extracted twice with EtOAc, and the combined organic phases were dried over sodium sulfate and concentrated in vacuo to give 6-chloro-5-[4-(1-methylpyrrolidin-3-yl)phenyl]-1H-indole-3-carbaldehyde (0.23 g, 16% yield) which was used directly in the next step. MS (ES+) 339.0 (M+H)+.

後処理

  1. customyielding a thick suspension
  2. temperatureThe resulting mixture was heated at 90° C. for 30 min
  3. temperatureThe reaction mixture was cooled
  4. custompartitioned between water and EtOAc
  5. extractionThe aqueous phase was extracted twice with EtOAc
  6. dry with materialthe combined organic phases were dried over sodium sulfate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0d660c52160d407ab2ca323f19e861c1
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889730B2

反応ノート

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