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Sodium borohydride → 3-Cycloheptyl-2-(4-methanesulfonyl-phenyl)-propionic acid methyl ester

HRID 430342
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 430342
[CH3:1][O:2][C:3](=[O:23])/[C:4](/[C:13]1[CH:18]=[CH:17][C:16]([S:19]([CH3:22])(=[O:21])=[O:20])=[CH:15][CH:14]=1)=[CH:5]/[CH:6]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[BH4-].[Na+]>CO.O.O.O.O.O.O.[Ni](Cl)Cl>[CH3:1][O:2][C:3](=[O:23])[CH:4]([C:13]1[CH:14]=[CH:15][C:16]([S:19]([CH3:22])(=[O:20])=[O:21])=[CH:17][CH:18]=1)[CH2:5][CH:6]1[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 4311764Sodium borohydrideHCID 67483512(E)-3-cycloheptyl-2-(4-methanesulfonyl-phenyl)-acrylic acid methyl ester

Produkt 1

HCID 544656743-Cycloheptyl-2-(4-methanesulfonyl-phenyl)-propionic acid methyl esterAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 11791229Dichloronickel;hexahydrateKatalysator
HCID 887
Methanol
Lösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of nickel(II) chloride hexahydrate (7.8 mg, 0.033 mmol) and (E)-3-cycloheptyl-2-(4-methanesulfonyl-phenyl)-acrylic acid methyl ester (111 mg, 0.33 mmol) in methanol (3 mL) was cooled to 0° C. and then treated with sodium borohydride (25 mg, 0.66 mmol) in two portions. After the addition, the black reaction mixture was stirred for 15 min at 0° C. and then allowed to warm to 25° C. where it was stirred for 15 h. The black solid was filtered using filter paper and washed with methanol. The combined solvents were concentrated in vacuo, and the residue was diluted with water (25 mL) and ethyl acetate (25 mL). The two layers were separated, and the aqueous layer was extracted with ethyl acetate (1×15 mL). The combined organic extracts were washed with a saturated aqueous sodium chloride solution (1×50 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to afford racemic 3-cycloheptyl-2-(4-methanesulfonyl-phenyl)-propionic acid methyl ester (101 mg, 91%) as a colorless oil: EI-HRMS m/e calcd for C18H26O4S (M+) 338.1552, found 338.1555.

Aufarbeitung

  1. additionAfter the addition
  2. temperatureto warm to 25° C. where it
  3. stirringwas stirred for 15 h
  4. filtrationThe black solid was filtered
  5. filtrationusing filter paper
  6. washwashed with methanol
  7. concentrationThe combined solvents were concentrated in vacuo
  8. additionthe residue was diluted with water (25 mL) and ethyl acetate (25 mL)
  9. customThe two layers were separated
  10. extractionthe aqueous layer was extracted with ethyl acetate (1×15 mL)
  11. washThe combined organic extracts were washed with a saturated aqueous sodium chloride solution (1×50 mL)
  12. dry with materialdried over anhydrous magnesium sulfate
  13. filtrationfiltered
  14. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-786f49db0df147bab2711b8f41f6fbe8
Quelldatensatz
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06320050B1

Notizen zur Reaktion

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