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3-Methoxypropylamine → Tert-butyl (3-((7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl)amino)propyl)(3-methoxypropyl)carbamate

HRID 1921980
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1921980
Br[CH2:2][CH2:3][CH2:4][NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[CH:9]=[C:8]([C:18]2[CH:23]=[CH:22][N:21]=[C:20]([NH:24][CH3:25])[N:19]=2)[CH:7]=1.[CH3:26][O:27][CH2:28][CH2:29][CH2:30][NH2:31].[C:32](=O)([O:38]C(C)(C)C)[O:33][C:34]([CH3:37])([CH3:36])[CH3:35].C(N(CC)CC)C>CN(C)C(=O)C>[CH3:17][O:16][C:13]1[CH:14]=[C:15]2[C:10]([CH:9]=[C:8]([C:18]3[CH:23]=[CH:22][N:21]=[C:20]([NH:24][CH3:25])[N:19]=3)[CH:7]=[C:6]2[NH:5][CH2:4][CH2:3][CH2:2][N:31]([CH2:30][CH2:29][CH2:28][O:27][CH3:26])[C:32](=[O:38])[O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[CH:11][CH:12]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 16723-MethoxypropylamineHCID 8471TriethylamineHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) esterHCID 532581654-(4-((3-bromopropyl)amino)-6-methoxynaphthalen-2-yl)-N-methylpyrimidin-2-amine

Produkt 1

HCID 67307853Tert-butyl (3-((7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl)amino)propyl)(3-methoxypropyl)carbamate
Ausbeute 39,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

A mixture of 4-(4-((3-bromopropyl)amino)-6-methoxynaphthalen-2-yl)-N-methylpyrimidin-2-amine (189) (0.10 g, 0.25 mmol) and N,N-dimethylacetamide (2 mL) were treated with 3-methoxypropan-1-amine (0.10 mL, 1.0 mmol). The resulting mixture was stirred at room temperature 16 h. The reaction mixture was dried down and treated with di-tert-butyl carbonate solution (1 mL of 0.6 M solution in methanol, 0.6 mmol) and triethylamine (0.5 mL, 3.6 mmol). The resulting mixture was stirred at room temperature for 16 h. The reaction mixture was concentrated (rotary) and dissolved in ethyl acetate (20 mL) and water (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organics were dried over Na2SO4, filtered and concentrated (rotary). The residue was purified by column chromatography (silica gel) using 85% ethyl acetate/hexanes as the eluent to afford tert-butyl (3-((7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl)amino)propyl)(3-methoxypropyl)carbamate (190) as an orange oil (0.05 g). The residue was dissolved in dioxane (1 mL) and then treated with HCl (4 M in dioxane, 0.5 mL, 7.2 mmol). The reaction mixture was stirred at room temperature and then filtered to afford N-{7-methoxy-3-[2-(methylamino)pyrimidin-4-yl]-1-naphthyl}-N′-(3-methoxypropyl)propane-1,3-diamine was isolated as a red-orange solid. M.p.=130-132° C. 400 MHz 1H NMR (DMSO-d6) δ: 8.88 (br s, 2H), 8.44 (d, J=6.3 Hz, 1H), 8.11 (br s, 1H), 7.90 (d, J=9.0 Hz, 1H), 7.66-7.56 (m, 2H), 7.28-7.24 (m, 2H), 3.96 (s, 3H), 3.56-3.41 (m, 4H), 3.22 (s, 3H), 3.20-2.95 (m, 7H); Experimental Elemental Analysis (3.2 equivalents of HCl)=52.49% C, 6.19% H, 12.82% N; Calculated Elemental Analysis 52.50% C, 6.55% H, 13.31% N; LCMS (m/z): 410 [M+H].

Aufarbeitung

  1. customThe reaction mixture was dried down
  2. stirringThe resulting mixture was stirred at room temperature for 16 h
  3. concentrationThe reaction mixture was concentrated (rotary)
  4. dissolutiondissolved in ethyl acetate (20 mL)
  5. extractionThe aqueous layer was extracted with ethyl acetate (2×10 mL)
  6. dry with materialThe combined organics were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated (rotary)
  9. customThe residue was purified by column chromatography (silica gel)

Quellen und Nachweise

ORD-Eintrag
ord-ac88514fcc75401e8891789eed6b13fb
Quelldatensatz
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08173808B2

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