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Hexane → 5-chloro-2'-pyridin-4-yl-6',7'-dihydro-3H,5'H-spiro[2-benzofuran-1,4'-[1]benzothiophen]-3-one

HRID 1615486
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1615486
[Cl:1][C:2]1[CH:3]=[CH:4][C:5](I)=[C:6]([CH:14]=1)[C:7](N(CC)CC)=[O:8].C([Li])CCC.CCCCCC.[N:27]1[CH:32]=[CH:31][C:30]([C:33]2[S:34][C:35]3[CH2:41][CH2:40][CH2:39][C:38](=[O:42])[C:36]=3[CH:37]=2)=[CH:29][CH:28]=1>O1CCCC1.CCOC(C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:38]3([O:42][C:7](=[O:8])[C:6]=2[CH:14]=1)[C:36]1[CH:37]=[C:33]([C:30]2[CH:31]=[CH:32][N:27]=[CH:28][CH:29]=2)[S:34][C:35]=1[CH2:41][CH2:40][CH2:39]3
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 8058HexaneHCID 121119092-pyridin-4-yl-6,7-dihydro-1-benzothiophen-4(5H)-oneHCID 681829545-chloro-N,N-diethyl-2-iodobenzamideHCID 178418339Butyllithium

Produkt 1

HCID 681829575-chloro-2'-pyridin-4-yl-6',7'-dihydro-3H,5'H-spiro[2-benzofuran-1,4'-[1]benzothiophen]-3-oneAusbeute 77,1 %

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 8028TetrahydrofuranLösungsmittel2×HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

In a 100 mL round bottomed flask was placed 5-chloro-N,N-diethyl-2-iodobenzamide (840 mg, 2.5 mmol) and tetrahydrofuran (10 mL). The mixture was stirred for 5 min at −78° C. then n-butyllithium in hexane (1.6M, 1.8 mL, 2.9 mmol) was added and the mixture was stirred for an additional 30 min at the same temperature. To the mixture was added a solution of 2-pyridin-4-yl-6,7-dihydro-1-benzothiophen-4(5H)-one (445 mg, 1.94 mmol) in tetrahydrofuran (15 mL). The mixture was stirred for an additional 16 hr during which time the reaction temperature was allowed to slowly rise from −78° C. to rt. The reaction mixture was then refluxed for 4 hr, cooled to rt and then diluted with EtOAc (50 mL). The resulting solution was washed with water (50 mL). The aqueous phase was separated and neutralized by the addition of 1N HCl (ca 1.21 mL, pH ca 7.0) and then extracted with EtOAc (50 mL). Finally, the combined organic phases were washed with brine (30 mL) then dried over anhydrous MgSO4. Insoluble materials were removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by pre-packed silica gel (40 g) column chromatography, eluting with 30% to 100% EtOAc/hexane to yield the title compound (550 mg; 77%) as an off-white foam, which included a small amount of 2-pyridin-4-yl-1-benzothiophene-4-ol as an impurity. The crude material was used in the next step without further purification. LCMS: (FA) ES+ 368, 370; 1H NMR (400 MHz, d6-DMSO) δ ppm 8.46 (dd, 2H), 7.98 (dd, 1H), 7.82 (dd, 1H), 7.57 (d, 1H), 7.49 (dd, 2H), 7.11 (s, 1H), 3.03-3.09 (m, 1H), 2.89-2.97 (m, 1H), 2.29-2.37 (m, 1H), 2.00-2.16 (m, 3H).

Aufarbeitung

  1. customIn a 100 mL round bottomed flask was placed
  2. stirringthe mixture was stirred for an additional 30 min at the same temperature
  3. stirringThe mixture was stirred for an additional 16 hr during which time the reaction temperature
  4. customto slowly rise from −78° C. to rt
  5. temperatureThe reaction mixture was then refluxed for 4 hr
  6. temperaturecooled to rt
  7. washThe resulting solution was washed with water (50 mL)
  8. customThe aqueous phase was separated
  9. additionneutralized by the addition of 1N HCl (ca 1.21 mL, pH ca 7.0)
  10. extractionextracted with EtOAc (50 mL)
  11. washFinally, the combined organic phases were washed with brine (30 mL)
  12. dry with materialthen dried over anhydrous MgSO4
  13. customInsoluble materials were removed by filtration
  14. concentrationthe filtrate was concentrated under reduced pressure
  15. customThe residue was purified by pre-packed silica gel (40 g) column chromatography
  16. washeluting with 30% to 100% EtOAc/hexane

Quellen und Nachweise

ORD-Eintrag
ord-058d628454b3456cac4aa745d99403d7
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08765746B2

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