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Triethylamine → 3-{(3-Benzyloxy-propyl)-[4-(4-chloro-benzenesulfonyl)-5,8-difluoro-chroman-3-yl]-amino}-propan-1-ol

HRID 564336
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 564336
Br[CH2:2][CH2:3][CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[NH2:13][CH2:14][CH2:15][CH2:16][OH:17].[Cl:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([C:28]2[C:37]3[C:32](=[C:33]([F:39])[CH:34]=[CH:35][C:36]=3[F:38])[O:31][CH2:30][CH:29]=2)(=[O:27])=[O:26])=[CH:21][CH:20]=1.C(N(CC)CC)C>C1COCC1>[CH2:6]([O:5][CH2:4][CH2:3][CH2:2][N:13]([CH:29]1[CH:28]([S:25]([C:22]2[CH:21]=[CH:20][C:19]([Cl:18])=[CH:24][CH:23]=2)(=[O:27])=[O:26])[C:37]2[C:32](=[C:33]([F:39])[CH:34]=[CH:35][C:36]=2[F:38])[O:31][CH2:30]1)[CH2:14][CH2:15][CH2:16][OH:17])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 90863-Amino-1-propanolHCID 2776064Benzyl 3-Bromopropyl EtherHCID 582522424-((4-Chlorophenyl)sulfonyl)-5,8-difluoro-2H-chromene

Produkt 1

HCID 670060863-{(3-Benzyloxy-propyl)-[4-(4-chloro-benzenesulfonyl)-5,8-difluoro-chroman-3-yl]-amino}-propan-1-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Benzyl 3-bromopropyl ether (7.8475 g, 34.27 mmol) was dissolved in 50 ml of THF then 3-aminopropanol (2.56 g, 34.13 mmol) was added the reaction was stirred at room temperature for three days. The reaction was quenched with 100 ml of Sat. potassium carbonate solution and the solution washed with ethyl acetate. The organic layer washed with Sat. potassium carbonate solution (2×100 mL) then dried over sodium sulfate and concentrated. This amine solution was used without any further purification. The amine solution (3.91 g, 17.5 mmol) was dissolved in 100 ml of THF. 4-(4-Chloro-benzenesulfonyl)-5,8-difluoro-2H-chromene (2.0486 g, 5.97 mmol) was added and the reaction was stirred at room temperature overnight. Triethylamine (3 ml) was added and the reaction was stirred at room temperature for 2 h. Then additional amine solution (2.85 g, 12.8 mmol) was added and the reaction was stirred overnight at room temperature then warmed to reflux and stirred overnight. The reaction was quenched with water (100 ml) and washed with ethyl acetate (100 ml). The organic layer was dried over sodium sulfate and concentrated. The product was purified by column using EtOAc/Hex. as the eluent (gradient from 0/100 to 100/0 in 45 minutes). Yield: 570 mg, 17%. 1H NMR (CDCl3 400 MHz) δ7.64-7.59 (m, 2H), 7.45-7.40 (m, 2H), 7.36-7.25 (m, 5H), 7.00 (td, J=9.5, 5.1 Hz, 1H), 6.42 (td, J=8.8, 3.7 Hz, 1H), 4.74 (dd, J=12.4, 5.1 Hz, 1H), 4.65 (s, 1H), 4.42 (s, 2H), 4.32-4.26 (m, 1H), 4.06-4.01 (m, 1H), 3.59 (t, J=5.4 Hz, 2H), 3.41 (t, J=5.9 Hz, 2H), 2.87 (bs, 1H), 2.71-2.53 (m, 3H), 2.50-2.42 (m, 1H), 1.74-1.62 (m, 3H), 1.60-1.50 (m, 1H).

Aufarbeitung

  1. customThe reaction was quenched with 100 ml of Sat. potassium carbonate solution
  2. washthe solution washed with ethyl acetate
  3. washThe organic layer washed with Sat. potassium carbonate solution (2×100 mL)
  4. dry with materialthen dried over sodium sulfate
  5. concentrationconcentrated
  6. customThis amine solution was used without any further purification
  7. stirringthe reaction was stirred at room temperature overnight
  8. stirringthe reaction was stirred at room temperature for 2 h
  9. stirringthe reaction was stirred overnight at room temperature
  10. temperaturethen warmed
  11. temperatureto reflux
  12. stirringstirred overnight
  13. customThe reaction was quenched with water (100 ml)
  14. washwashed with ethyl acetate (100 ml)
  15. dry with materialThe organic layer was dried over sodium sulfate
  16. concentrationconcentrated
  17. customThe product was purified by column
  18. customas the eluent (gradient from 0/100 to 100/0 in 45 minutes)

Quellen und Nachweise

ORD-Eintrag
ord-659d83bf3d474e18808ebeb3916e1893
Quelldatensatz
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08067621B2

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