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Sodium Carbonate → 6-Chloro-5-(4-methoxyphenyl)-1H-indole

HRID 1054841
ノート
印刷プレビュー

反応式

HRID 1054841 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]=[CH:5]2.C(=O)([O-])[O-].[Na+].[Na+].[CH3:18][O:19][C:20]1[CH:25]=[CH:24][C:23](B(O)O)=[CH:22][CH:21]=1.[NH4+].[Cl-]>CCO.C1(C)C=CC=CC=1.O.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>[Cl:11][C:10]1[CH:9]=[C:8]2[C:4]([CH:5]=[CH:6][NH:7]2)=[CH:3][C:2]=1[C:23]1[CH:24]=[CH:25][C:20]([O:19][CH3:18])=[CH:21][CH:22]=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

9

反応物 4

HCID 10340Sodium CarbonateHCID 25517Ammonium ChlorideHCID 201262(4-Methoxyphenyl)boronic acidHCID 144196195-Bromo-6-chloro-1H-indole

生成物 1

HCID 866986576-Chloro-5-(4-methoxyphenyl)-1H-indole収率 39.1%

試薬・触媒・溶媒 4

HCID 178418397
HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

A mixture of 5-bromo-6-chloro-1H-indole (3.20 g, 13.9 mmol), sodium carbonate (3.68 g, 34.7 mmol), and 4-methoxyphenylboronic acid (2.41 g, 15.9 mmol) in EtOH (18 mL), toluene (18 mL) and water (18 mL) was degassed with N2 for 15 minutes, treated with tetrakis(triphenylphosphine)palladium(0) (1.20 g, 0.99 mmol) and heated to 90° C. for 23 hours. The cooled reaction mixture was poured into half-saturated NH4Cl solution (200 mL) and extracted with dichloromethane (3×120 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The resulting dark solid was purified by flash chromatography (5-20% EtOAc/heptane) to give the title compound (1.40 g, 39%) as a white solid. MS (ES+) 258.5 (M+H)+. 1H NMR (500 MHz, CDCl3) δ 8.16 (br. s., 1 H), 7.56 (s, 1 H), 7.42 (d, J=8.1 Hz, 2 H), 7.24 (s, 1 H), 6.98 (d, J=8.1 Hz, 2 H), 6.55 (br. s., 1 H), 3.88 (s, 3 H).

後処理

  1. customwas degassed with N2 for 15 minutes
  2. customThe cooled reaction mixture
  3. extractionextracted with dichloromethane (3×120 mL)
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe resulting dark solid was purified by flash chromatography (5-20% EtOAc/heptane)

出典と根拠

ORDレコード
ord-257bba41205045a39d04387a345818cb
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394285B2

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