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Sulfuric acid magnesium salt (1:1) → tert-Butyl 3-methyl-1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate

HRID 1501756
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1501756
O=[C:2]([CH3:21])[CH2:3][C:4]1([C:17](OC)=[O:18])[CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]1.C([O-])(=O)C.[NH4+].C([BH3-])#[N:28].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>CO>[CH3:21][CH:2]1[CH2:3][C:4]2([CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]2)[C:17](=[O:18])[NH:28]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 867094441-Tert-butyl 4-methyl 4-(2-oxopropyl)piperidine-1,4-dicarboxylate

Produkt 1

HCID 86709445tert-Butyl 3-methyl-1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

1-tert-Butyl 4-methyl 4-(2-oxopropyl)piperidine-1,4-dicarboxylate (1.15 g, 3.84 mmol) in methanol (25 mL) was treated with ammonium acetate (3.85 g, 49.9 mmol), sodium cyanoborohydride (0.681 g, 10.83 mmol) and magnesium sulfate (2.54 g, 21.1 mmol). The mixture was heated at 80° C. in a sealed tube for 12 hours. The reaction mixture was filtered through a pad of CELITE® and the filter cake was washed with methanol. The filtrates were then concentrated and the residue was purified by column chromatography eluting with 0-10% methanol/ethyl acetate to afford the title compound. LC-MS (IE, m/z): 291.27 (M+23)+

Aufarbeitung

  1. filtrationThe reaction mixture was filtered through a pad of CELITE®
  2. washthe filter cake was washed with methanol
  3. concentrationThe filtrates were then concentrated
  4. customthe residue was purified by column chromatography
  5. washeluting with 0-10% methanol/ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-8526817832b543d49fba645f767f5fdd
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09206198B2

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