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Potassium Carbonate → 6-chloro-5-(3-methoxyphenyl)-1H-indole-3-carbaldehyde

HRID 338300
ノート
印刷プレビュー

反応式

HRID 338300 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[NH:7][CH:6]=[C:5]2[CH:12]=[O:13].[CH3:14][O:15][C:16]1[CH:17]=[C:18](B(O)O)[CH:19]=[CH:20][CH:21]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.CN(C=O)C.O>[Cl:11][C:10]1[CH:9]=[C:8]2[C:4]([C:5]([CH:12]=[O:13])=[CH:6][NH:7]2)=[CH:3][C:2]=1[C:20]1[CH:19]=[CH:18][CH:17]=[C:16]([O:15][CH3:14])[CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 2734370(3-Methoxyphenyl)boronic acidHCID 866985665-bromo-6-chloro-1H-indole-3-carbaldehyde

生成物 1

HCID 866986466-chloro-5-(3-methoxyphenyl)-1H-indole-3-carbaldehyde収率 52.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 21712069
1,4-dioxane N,N-dimethylformamide
溶媒

実験手順

To a solution of 5-bromo-6-chloro-1H-indole-3-carbaldehyde (300 mg, 2 mmol) in dioxane/DMF=1/1 (4 mL) was added (3-methoxyphenyl)boronic acid (463 mg, 1.8 mmol), potassium carbonate (828 mg, 6 mmol) in water (1 mL), and Pd (dppf)Cl2 (50 mg) in a microwave vial. The sealed vial was irradiated in the microwave on a Biotage Smith Synthesizer at 110° C. for 30 min, TLC (petroleum ether/ethyl acetate=1:1) showed the reaction was complete. The solvent was removed in vacuo and the mixture was partitioned between ethyl acetate and water. The combined organics were dried over sodium sulfate, concentrated in vacuo, and purified by combi-flash to give the title compound (270 mg, 47%) as a yellow solid

後処理

  1. customThe sealed vial was irradiated in the microwave on a Biotage Smith Synthesizer at 110° C. for 30 min
  2. customThe solvent was removed in vacuo
  3. customthe mixture was partitioned between ethyl acetate and water
  4. dry with materialThe combined organics were dried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. custompurified by combi-flash

出典と根拠

ORDレコード
ord-49dda996d4504186a69df8c4143ffaaf
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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