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1-Propanol → HCID 24743834, 화합물

HRID 641867
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HRID 641867 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3](B(O)O)[CH:2]=1.Br[C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[N:16]([S:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)(=[O:22])=[O:21])[CH:15]=[C:14]2[C:29]1[CH2:30][CH2:31][N:32]([CH3:35])[CH2:33][CH:34]=1.C(O)CC.C([O-])([O-])=O.[Na+].[Na+]>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>[CH3:35][N:32]1[CH2:33][CH:34]=[C:29]([C:14]2[C:13]3[C:17](=[CH:18][CH:19]=[C:11]([C:4]4[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=4)[CH:12]=3)[N:16]([S:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)(=[O:22])=[O:21])[CH:15]=2)[CH2:30][CH2:31]1
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참가 물질

7

반응물 4

HCID 10311-PropanolHCID 10340Sodium CarbonateHCID 27343783-Pyridinylboronic acidHCID 534150661-(benzenesulfonyl)-5-bromo-3-(1-methyl-3,6-dihydro-2H-pyridin-4-yl)indole

생성물 1

HCID 24743834HCID 24743834, 화합물수율 43.1%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 962Water용매

실험 절차

Into a 100 mL 3-necked round bottom flask was placed pyridin-3-ylboronic acid (200 mg, 1.63 mmol), 5-bromo-3-(1-methyl-1,2,3,6-tetrahydropyridin-4-yl)-1-(phenylsulfonyl)-1H-indole (470 mg, 1.08 mmol), and n-propanol (140 mL). The mixture was stirred at room temperature for 30 min during which time the solids dissolved. A solution of Na2CO3 (430 mg, 4.06 mmol) in water (5 mL) was then added, followed by the addition of Pd(PPh3)4 (130 mg, 0.108 mmol). The resulting solution was stirred at reflux temperature overnight, and then concentrated. The residue was dissolved in water (10 mL), and the resulting solution was extracted diethylether (2×50 mL). The organic layers were combined and the residue was purified by column chromatography using a 1:5 dichloromethane/methanol solvent system to afford 200 mg (42.5%) of 3-(1-methyl-1,2,3,6-tetrahydropyridin-4-yl)-1-(phenylsulfonyl)-5-(pyridin-4-yl)-1H-indole as a deep yellow solid. 1H NMR (CDCl3) δ 8.69 (d, 2H), 8.12 (d, 1H), 7.93 (t, 3H), 7.60 (d, 3H), 7.48 (d×d, 4H), 6.18 (s, 1H), 2.85 (2H), 1.52 (2H), 1.25 (3H), 0.87 (2H). LC/MS (EI) tR 2.18, m/z 430.0 (M++1)

후처리

  1. customInto a 100 mL 3-necked round bottom flask was placed
  2. dissolutiondissolved
  3. stirringThe resulting solution was stirred
  4. temperatureat reflux temperature overnight
  5. concentrationconcentrated
  6. dissolutionThe residue was dissolved in water (10 mL)
  7. extractionthe resulting solution was extracted diethylether (2×50 mL)
  8. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-c436c1a9fcae416385e30e8c5e688755
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07696229B2

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