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Potassium Carbonate → tert-butyl 5-bromo-3-(quinolin-3-yl)-1H-indole-1-carboxylate

HRID 634147
ノート
印刷プレビュー

反応式

HRID 634147 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH:6]=[C:5]2I.[N:19]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:22]=[C:21](B(O)O)[CH:20]=1.C(=O)([O-])[O-].[K+].[K+].C([O-])(O)=O.[Na+]>O1CCOCC1.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.O>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH:6]=[C:5]2[C:21]1[CH:20]=[N:19][C:28]2[C:23]([CH:22]=1)=[CH:24][CH:25]=[CH:26][CH:27]=2
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

8

反応物 4

HCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 2734663Quinoline-3-boronic acidHCID 17749978tert-butyl 5-bromo-3-iodo-1H-indole-1-carboxylate

生成物 1

HCID 68327989tert-butyl 5-bromo-3-(quinolin-3-yl)-1H-indole-1-carboxylate収率 36.6%

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

To a mixture of tert-butyl 5-bromo-3-iodo-1H-indole-1-carboxylate (1.750 g, 4.146 mmol, synchem), 3-quinolineboronic acid (1.076 g, 6.22 mmol), Pd(PPh3)4 (0.240 g, 0.207 mmol) and potassium carbonate ((1.719 g, 12.439 mmol) in dioxane (3.0 mL) was added H2O (1.0 mL) and the reaction was heated at 60° C. for 42 h. Saturated NaHCO3 solution (5.0 mL) was added to the mixture. The resulting mixture was extracted with EtOAc. The organic phases were combined, dried with sodium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography to give tert-butyl 5-bromo-3-(quinolin-3-yl)-1H-indole-1-carboxylate (642 mg, 36.6%) as a white foam. MS (ESI, pos. ion) m/z: 423 (M+1); 1H NMR (400 MHz, DMSO-d6) δ ppm 1.68 (s, 9H), 7.62 (dd, J=8.8, 1.8 Hz, 1H), 7.67 (t, J=7.8 Hz, 1H), 7.79 (t, J=7.3 Hz, 1H), 8.07 (d, J=8.5 Hz, 1H), 8.13-8.20 (m, 3H), 8.30 (s, 1H), 8.74 (d, J=1.5 Hz, 1H), 9.26 (d, J=2.0 Hz, 1H)

後処理

  1. extractionThe resulting mixture was extracted with EtOAc
  2. dry with materialdried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-50843f9ab0d74475a693b699815508de
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321756B2

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