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Thionyl Chloride → 3-(4-Isobutyl-3-(trifluoromethyl)phenyl)-7-vinyl-4,5-dihydronaphtho[1,2-c]isoxazole

HRID 1506368
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1506368
[Li+].CC([N-]C(C)C)C.[CH:9]([C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][CH:20]=1)/[C:17](=[N:21]/[OH:22])/[CH2:16][CH2:15][CH2:14]2)=[CH2:10].[CH2:23]([C:27]1[CH:36]=[CH:35][C:30]([C:31](OC)=O)=[CH:29][C:28]=1[C:37]([F:40])([F:39])[F:38])[CH:24]([CH3:26])[CH3:25].S(Cl)(Cl)=O>C1COCC1.N1C=CC=CC=1>[CH2:23]([C:27]1[CH:36]=[CH:35][C:30]([C:31]2[O:22][N:21]=[C:17]3[C:18]4[C:13]([CH2:14][CH2:15][C:16]=23)=[CH:12][C:11]([CH:9]=[CH2:10])=[CH:20][CH:19]=4)=[CH:29][C:28]=1[C:37]([F:38])([F:39])[F:40])[CH:24]([CH3:26])[CH3:25]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 24386Thionyl ChlorideHCID 2724682Lithium diisopropylamideHCID 58020990Methyl 4-isobutyl-3-(trifluoromethyl)benzoateHCID 121012766(NE)-N-(6-ethenyl-3,4-dihydro-2H-naphthalen-1-ylidene)hydroxylamine2×

Produkt 1

HCID 671691843-(4-Isobutyl-3-(trifluoromethyl)phenyl)-7-vinyl-4,5-dihydronaphtho[1,2-c]isoxazole
Ausbeute 57,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineKatalysatorHCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To the LDA solution was added 6-vinyl-3,4-dihydronaphthalen-1(2H)-one oxime (Intermediate 1, 0.25 g, 1.335 mmol) dissolved in 1 mL of THF dropwise over a period of 1 min. at 0° C. After 15 min., methyl 4-isobutyl-3-(trifluoromethyl)benzoate (Preparation 23B, 0.347 g, 1.335 mmol) dissolved in 1 mL of THF was added dropwise over a period of 1 min. at 0° C. and the contents were stirred at 0° C. for 10 min. The reaction mixture was partitioned between 1N hydrochloric acid (5 mL) and ethyl acetate (10 mL)-THF. The 1N hydrochloric acid layer was back extracted with ethyl acetate (10 mL). The combined ethyl acetate layers were dried over sodium sulfate and concentrated under reduced pressure. The resulting yellow solid was azeotroped with toluene (5 mL). To the solid was added toluene (5.00 mL), followed by thionyl chloride (0.195 mL, 2.67 mmol) and 1 drop of pyridine. The contents were heated at 110° C. for 5 min. The dark reaction mixture was concentrated and partitioned between ethyl acetate (15 mL) and water (10 mL). The ethyl acetate layer was dried over sodium sulfate, concentrated and subjected to silica gel column chromatography (hexane/ethyl acetate). Fractions corresponding to the product were collected and concentrated to yield 3-(4-isobutyl-3-(trifluoromethyl)phenyl)-7-vinyl-4,5-dihydronaphtho[1,2-c]isoxazole (0.305 g, 0.767 mmol, 57.5% yield) as a pale yellow solid.

Aufarbeitung

  1. additionwas added dropwise over a period of 1 min. at 0° C.
  2. customThe reaction mixture was partitioned between 1N hydrochloric acid (5 mL) and ethyl acetate (10 mL)-THF
  3. extractionThe 1N hydrochloric acid layer was back extracted with ethyl acetate (10 mL)
  4. dry with materialThe combined ethyl acetate layers were dried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting yellow solid was azeotroped with toluene (5 mL)
  7. additionTo the solid was added toluene (5.00 mL)
  8. temperatureThe contents were heated at 110° C. for 5 min
  9. customThe dark reaction mixture
  10. concentrationwas concentrated
  11. custompartitioned between ethyl acetate (15 mL) and water (10 mL)
  12. dry with materialThe ethyl acetate layer was dried over sodium sulfate
  13. concentrationconcentrated
  14. customFractions corresponding to the product were collected
  15. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-c273349b52264d26a438231810d10084
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09216972B2

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