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Potassium Carbonate → 4,6-Difluoro-5-(4-(1-hydroxycyclobutyl)phenyl)-1H-indole-3-carbaldehyde

HRID 1054574
ノート
印刷プレビュー

反応式

HRID 1054574 の反応式
CC1(C)COB(B2OCC(C)(C)CO2)OC1.C([O-])(=O)C.[K+].Br[C:23]1[CH:28]=[CH:27][C:26]([C:29]2([OH:33])[CH2:32][CH2:31][CH2:30]2)=[CH:25][CH:24]=1.Br[C:35]1[C:36]([F:47])=[C:37]2[C:41](=[CH:42][C:43]=1[F:44])[NH:40][CH:39]=[C:38]2[CH:45]=[O:46].C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.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].CCO.C1(C)C=CC=CC=1>[F:47][C:36]1[C:35]([C:23]2[CH:28]=[CH:27][C:26]([C:29]3([OH:33])[CH2:32][CH2:31][CH2:30]3)=[CH:25][CH:24]=2)=[C:43]([F:44])[CH:42]=[C:41]2[C:37]=1[C:38]([CH:45]=[O:46])=[CH:39][NH:40]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

10

反応物 5

HCID 11430Potassium CarbonateHCID 517044Potassium AcetateHCID 2734316Bis(neopentyl glycolato)diboronHCID 120954191-(4-Bromophenyl)cyclobutanolHCID 866985785-Bromo-4,6-difluoro-1H-indole-3-carbaldehyde

生成物 1

HCID 866985794,6-Difluoro-5-(4-(1-hydroxycyclobutyl)phenyl)-1H-indole-3-carbaldehyde
収率 66.5%

試薬・触媒・溶媒 4

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒2 回HCID 702Ethanol溶媒HCID 1140Toluene溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
110 °C

実験手順

A mixture of 5,5,5′,5′-tetramethyl-2,2′-bi(1,3,2-dioxaborinane) (188.0 mg, 0.55 mmol), oven dried potassium acetate (230.0 mg, 2.34 mmol), and 1-(4-bromophenyl)cyclobutanol (114.0 mg, 0.50 mmol) in 1,4-dioxane (2 mL) was degassed with N2 for 15 min, then treated with [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (20.0 mg, 0.027 mmol). The reaction mixture was subjected to microwave irradiation at 110° C. for 1 hour. The cooled reaction mixture was filtered through celite, rinsed with EtOAc and concentrated to dryness. To the resulting dark solid ((45.0 mg, 0.17 mmol) was added 5-bromo-4,6-difluoro-1H-indole-3-carbaldehyde (45.0 mg, 0.17 mmol), 2 N aqueous potassium carbonate (0.20 mL, 0.40 mmol), toluene (1.5 mL) and EtOH (0.5 mL). The reaction mixture was degassed with N2 for 10 minutes, treated with [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (14.0 mg, 0.019 mmol), and heated in a sealed pressure tube at 110° C. for 2 hours. The reaction mixture was cooled to room temperature and purified by flash chromatography (0-67% EtOAc/heptanes) to give the title compound (37 mg, 65%) as a white solid. MS (ES+) 328.0 (M+H)+. 1H NMR (500 MHz, CD3OD) δ 10.04 (d, J=2.68 Hz, 1 H), 8.15 (s, 1 H), 7.64 (d, J=8.05 Hz, 2 H), 7.48 (d, J=8.05 Hz, 2 H), 7.21 (d, J=9.51 Hz, 1 H), 2.57-2.66 (m, 2 H), 2.39-2.46 (m, 2 H), 2.03-2.12 (m, 1 H), 1.73-1.83 (m, 1 H).

後処理

  1. customwas degassed with N2 for 15 min
  2. customirradiation at 110° C. for 1 hour
  3. customThe cooled reaction mixture
  4. filtrationwas filtered through celite
  5. washrinsed with EtOAc
  6. concentrationconcentrated to dryness
  7. customThe reaction mixture was degassed with N2 for 10 minutes
  8. temperatureThe reaction mixture was cooled to room temperature
  9. custompurified by flash chromatography (0-67% EtOAc/heptanes)

出典と根拠

ORDレコード
ord-1f851abb00684c958da9bba46a587d7f
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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