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Toluene → 8-(6-(((2,6-diisopropylphenyl)amino)methyl)pyridin-2-yl)-N-phenyl-1,2,3,4-tetrahydronaphthalen-1-amine

HRID 928638
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 928638
C([O-])([O-])=O.[Na+].[Na+].C[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][CH:15]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][C:23]=2B2OC(C)(C)C(C)(C)O2)[CH2:18][CH2:17][CH2:16]1.Br[C:35]1[N:40]=[C:39]([CH2:41][NH:42][C:43]2[C:48]([CH:49]([CH3:51])[CH3:50])=[CH:47][CH:46]=[CH:45][C:44]=2[CH:52]([CH3:54])[CH3:53])[CH:38]=[CH:37][CH:36]=1.C1(C)C=CC=CC=1>O.CO.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>[CH:52]([C:44]1[CH:45]=[CH:46][CH:47]=[C:48]([CH:49]([CH3:51])[CH3:50])[C:43]=1[NH:42][CH2:41][C:39]1[N:40]=[C:35]([C:23]2[CH:22]=[CH:21][CH:20]=[C:19]3[C:24]=2[CH:15]([NH:14][C:9]2[CH:8]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:16][CH2:17][CH2:18]3)[CH:36]=[CH:37][CH:38]=1)([CH3:54])[CH3:53]
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Komponenten

8

Edukt 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 90311811N-[(6-Bromopyridin-2-yl)methyl]-2,6-diisopropylanilineHCID 123397142N-(2-methylphenyl)-8-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,4-tetrahydronaphthalen-1-amine

Produkt 1

HCID 1180726038-(6-(((2,6-diisopropylphenyl)amino)methyl)pyridin-2-yl)-N-phenyl-1,2,3,4-tetrahydronaphthalen-1-amine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418397HCID 178418397, VerbindungKatalysatorHCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A solution of 3.60 g (34.0 mmol) of Na2CO3 in a mixture of 150 ml of water and 45 ml of methanol was purged with argon for 30 min. The obtained solution was added to a mixture of 5.00 g (14.0 mmol) of N-(2-methylphenyl)-8-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,4-tetrahydronaphthalen-1-amine, 4.85 g (14.0 mmol) of N-[(6-bromopyridin-2-yl)methyl]-2,6-diisopropylaniline, 0.80 g (0.70 mmol) of Pd(PPh3)4, and 180 ml of toluene in argon atmosphere. This mixture was stirred for 12 h at 70° C. and then cooled to room temperature. The organic layer was separated, the aqueous layer was extracted with 3×50 ml of ethyl acetate. The combined organic extract was washed with brine, dried over Na2SO4, and evaporated to dryness. The residue was purified by flash chromatography on silica gel 60 (40-63 um, eluent: hexane-ethyl acetate-triethylamine=100:10:1, vol.). Yield 2.50 g (36%) of a yellow oil. Anal. Calc. for C35H41N3: C, 83.45; H, 8.20; N, 8.34. Found: C, 83.69; H, 8.08; N, 8.13.1H NMR (CDCl3): δ 7.62-7.63 (m, 1H, 7-H in tetrahydronaphtalene); 7.55-7.58 (m, 1H, 4-H in Py); 7.52-7.54 (m, 1H, 3-H in Py); 7.41-7.44 (m, 1H, 6-H in tetrahydronaphtalene); 7.37-7.39 (m, 1H, 5-H in Py); 7.15-7.16 (m, 1H, 5-H in tetrahydronaphtalene); 7.03-7.10 (m, 4H, 3,4,5-H in 2,6-diisopropylphenyl and 5-H in 2-methylphenyl); 6.93 (m, 1H, 3-H in 2-methylphenyl); 6.70 (m, 1H, 6-H in 2-methylphenyl); 6.59 (m, 1H, 4-H in 2-methylphenyl); 5.35 (m, 1H, 1-H in tetrahydronaphtalene); 3.94-4.03 (m, 2H, CH2); 3.92-3.94 (m, 1H, 4- or 4′-H in tetrahydronaphtalene); 3.68-3.70 (m, 1H, 4′- or 4-H in tetrahydronaphtalene); 3.30 (sept, J=6.8 Hz, 2H, CH in 2,6-diisopropylphenyl); 3.16-3.24 (m, 1H, 3- or 3′-H in tetrahydronaphtalene); 2.92-3.00 (m, 1H, 3′- or 3-H in tetrahydronaphtalene); 2.38-2.47 (m, 1H, 2- or 2′-H in tetrahydronaphtalene); 2.14-2.22 (m, 1H, 2′- or 2-H in tetrahydronaphtalene); 1.75 (s, 3H, CH3 in 2-methylphenyl); 1.18-1.22 (m, 12H, CH3 in 2,6-diisopropylphenyl).

Aufarbeitung

  1. customwas purged with argon for 30 min
  2. temperaturecooled to room temperature
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with 3×50 ml of ethyl acetate
  5. extractionThe combined organic extract
  6. washwas washed with brine
  7. dry with materialdried over Na2SO4
  8. customevaporated to dryness
  9. customThe residue was purified by flash chromatography on silica gel 60 (40-63 um, eluent: hexane-ethyl acetate-triethylamine=100:10:1, vol.)

Quellen und Nachweise

ORD-Eintrag
ord-2c4af402ff684843bf8a954149784cdf
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09290519B2

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