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Acetic Acid → 4-[2-(2,2-Dimethyl-4,6-dioxo-[1,3]dioxan-5-yl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester

HRID 29751
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 29751
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=[O:5])[O:3]1.[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][CH:21]([CH2:24][CH:25]=O)[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12].C(O)(=O)C.N1CCCCC1.[BH4-].[Na+].Cl>ClCCl.COC(C)(C)C>[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][CH:21]([CH2:24][CH2:25][CH:6]2[C:7](=[O:8])[O:9][C:2]([CH3:10])([CH3:1])[O:3][C:4]2=[O:5])[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 8082PiperidineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 4311764Sodium borohydrideHCID 10353694tert-Butyl 4-(2-oxoethyl)piperidine-1-carboxylate

Produkt 1

HCID 68508700
4-[2-(2,2-Dimethyl-4,6-dioxo-[1,3]dioxan-5-yl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester
Ausbeute 66,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 15413tert-Butyl methyl etherLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of meldrums acid (1.68 g, 11.66 mmol) and 4-(2-oxo-ethyl)-piperidine-1-carboxylic acid tert-butyl ester (2.21 g, 9.72 mmol) in dichloromethane (40 mL) was added acetic acid (0.055 mL, 0.972 mmol) and piperidine (0.096 mL, 0.972 mmol). The mixture was heated at reflux for 3 h, and then allowed to attain room temperature. After being diluted with tert-butyl methyl ether, the mixture was washed with NaHCO3 (sat.) and brine. The organic phase was dried, filtered and concentrated. The residue was dissolved in a mixture of EtOH (40 mL) and acetic acid (20 mL). The solution was cooled to 0° C., and NaBH4 (0.554 g, 14.6 mmol) was added in portions after which the solution was allowed to stir for 30 min at rt and then acidified to pH 3 with 1 M HCl. The solution was extracted several times with dichloromethane. The combined organic phases were dried, filtered, concentrated and filtered through a pad of silica gel (dichloromethane). The solvent was evaporated to give 4-[2-(2,2-Dimethyl-4,6-dioxo-[1,3]dioxan-5-yl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester as a colorless oil (2.30 g, 65%) which solidified on standing.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 3 h
  3. customto attain room temperature
  4. washthe mixture was washed with NaHCO3 (sat.) and brine
  5. customThe organic phase was dried
  6. filtrationfiltered
  7. concentrationconcentrated
  8. dissolutionThe residue was dissolved in a mixture of EtOH (40 mL) and acetic acid (20 mL)
  9. extractionThe solution was extracted several times with dichloromethane
  10. customThe combined organic phases were dried
  11. filtrationfiltered
  12. concentrationconcentrated
  13. filtrationfiltered through a pad of silica gel (dichloromethane)
  14. customThe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-86baea5576f147ec9e8b1b1bc871edf2
Quelldatensatz
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07423012B2

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