StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Triphenylphosphine → 2-(4-(4-Hydroxybutyl)phenyl methyl)thio 3-methyl chromen-4-one

HRID 1723985
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1723985
[SH:1][C:2]1[O:3][C:4]2[C:9]([C:10](=[O:12])[CH:11]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2.O[CH2:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21][CH2:22][CH2:23][CH2:24][OH:25])=[CH:17][CH:16]=1.[CH:26]1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C>C1COCC1.O>[OH:25][CH2:24][CH2:23][CH2:22][CH2:21][C:18]1[CH:19]=[CH:20][C:15]([CH2:14][S:1][C:2]2[O:3][C:4]3[C:9]([C:10](=[O:12])[C:11]=2[CH3:26])=[CH:8][CH:7]=[CH:6][CH:5]=3)=[CH:16][CH:17]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 124752772-Mercapto-chromen-4-oneHCID 177561734-(4-Hydroxymethyl-phenyl)-butan-1-ol

Produkt 1

HCID 177558312-(4-(4-Hydroxybutyl)phenyl methyl)thio 3-methyl chromen-4-oneAusbeute 46,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To solution of 2-mercapto-chromen-4-one (1.52 g, 7.90 mmol) and 4-(4-hydroxymethyl-phenyl)-butan-1-ol (1.90 g, 9.90 mmol) dissolved in anhydrous THF (80 mL) was added solid PPh3 (3.11 g, 11.90 mmol) and DIAD (2.30 mL, 11.90 mmol). After completion of addition the reaction mixture continued to stir at room temperature. After 20 hours, the reaction mixture was diluted with water. The aqueous layer was separated and extracted with ethyl acetate (3×). All combined organic layers were dried over Na2SO4, filtered, and concentrated to yield an oil. The crude material was purified using silica gel chromatography (1:1 pentane: ethyl acetate) to yield 2-[4-(4-hydroxy-butyl)-benzylsulfanyl]-3-methyl-chromen-4-one (1.29 g, 3.64 mmol) in moderate yield (46%). 1H (CDCl3, 600 MHz): δ 8.18 (1H, dd, J=7.9, 1.3 Hz), 7.60 (1H, ddd, J=8.6, 7.2, 1.7 Hz), 7.31 (2H, t, J=8.5 Hz), 7.29 (2H, d, J=8.1 Hz), 7.12 (2H, d, J=8.1 Hz), 4.36 (2H, s), 3.62 (2H, m), 2.61 (2H, t, J=7.5 Hz), 2.00 (3H, s),1.67 (2H, m), 1.56 (2H, m); 13C (CDCl3, 150 MHz): δ 174.9, 161.3, 156.0, 141.5, 133.2, 132.3, 128.3, 128.2, 125.7, 124.5, 122.2, 117.2, 116.3, 62.3, 34.7, 31.8, 29.2, 26.9, 10.1.; HRMS calcd for C21H22O3S 355.1363:, found 355.1364

Aufarbeitung

  1. additionAfter completion of addition the reaction mixture
  2. customThe aqueous layer was separated
  3. extractionextracted with ethyl acetate (3×)
  4. dry with materialAll combined organic layers were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto yield an oil
  8. customThe crude material was purified

Quellen und Nachweise

ORD-Eintrag
ord-db9374045d56418cad04c541963cad14
Quelldatensatz
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07485283B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion