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Sodium Carbonate → 1h-Indole,2-methyl-5-phenyl-1-(phenylsulfonyl)-

HRID 400613
ノート
印刷プレビュー

反応式

HRID 400613 の反応式
[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][C:15](Br)=[CH:16][CH:17]=3)[CH:12]=[C:11]2[CH3:20])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:21]1(B(O)O)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.[OH-].[NH4+].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][C:15]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)=[CH:16][CH:17]=3)[CH:12]=[C:11]2[CH3:20])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 10340Sodium CarbonateHCID 66827Phenylboronic AcidHCID 152568981-benzenesulfonyl-5-bromo-2-methyl-1H-indole

生成物 1

HCID 600264171h-Indole,2-methyl-5-phenyl-1-(phenylsulfonyl)-収率 91.1%

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒
HCID 702
Ethanol
溶媒
HCID 1140Toluene溶媒
HCID 14923Ammonium Hydroxide溶媒

実験手順

A mixture of 1-benzenesulfonyl-5-bromo-2-methyl-1H-indole (810 mg, 2.31 mmol), phenylboronic acid (850 mg, 6.97 mmol) and tetrakis(triphenylphosphine)palladium(0) (55 mg, 0.029 mmol) in 20 mL of toluene, 10 mL of ethanol, and 5 mL of 2 M sodium carbonate was warmed at reflux for 4 hours. The reaction was monitored by TLC (ethyl acetate-hexanes (5:95), 2× developed; and toluene-hexanes (1:1)) indicating a slightly more polar product. The mixture was cooled and diluted with 12% aqueous ammonium hydroxide solution and extracted with three 15 mL portions of ethyl acetate. The combined organic layers were washed with three 15 mL portions of brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude mixture was adsorbed onto silica gel and chromatographed on silica gel using ethyl acetate-hexanes (1:99, then 2:98, then 3:97) to afford 731 mg (91% yield) of 1-benzenesulfonyl-2-methyl-5-phenyl-1H-indole.

後処理

  1. temperaturewas warmed
  2. temperatureat reflux for 4 hours
  3. temperatureThe mixture was cooled
  4. extractionextracted with three 15 mL portions of ethyl acetate
  5. washThe combined organic layers were washed with three 15 mL portions of brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customchromatographed on silica gel

出典と根拠

ORDレコード
ord-56869d8437494037a97fbf4ed767859a
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08741897B2

反応ノート

読み込み中…

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