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Lithium aluminum hydride → (1R,3S,4S)-2-azabicyclo(2.2.1)heptan-3-ylmethanol

HRID 60251
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 60251
Cl.[C@H:2]12[CH2:8][C@H:5]([CH2:6][CH2:7]1)[C@@H:4]([C:9](O)=[O:10])[NH:3]2.[AlH4-].[Li+]>O1CCCC1>[C@H:2]12[CH2:8][C@H:5]([CH2:6][CH2:7]1)[C@@H:4]([CH2:9][OH:10])[NH:3]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 28112Lithium aluminum hydrideHCID 20849996(1R,3S,4S)-2-azabicyclo[2.2.1]heptane-3-carboxylic acid hydrochloride

Produkt 1

HCID 11480448(1R,3S,4S)-2-azabicyclo(2.2.1)heptan-3-ylmethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a slurry of (1R,3S,4S)-2-azabicyclo[2.2.1]heptane-3-carboxylic acid hydrogen chloride (500 mg, 3 mmol) in tetrahydrofuran (4.6 mL) was added lithium tetrahydroaluminate (1N solution in tetrahydrofuran, 5.7 mL, 6 mmol) dropwise over 10 minutes. The reaction mixture was stirred overnight at ambient temperature under an atmosphere of nitrogen. The reaction was quenched with a few drops of water, diluted with diethyl ether (50 mL) and tetrahydrofuran (25 mL). The reaction mixture was basified to a pH of ˜11 by the addition of potassium hydroxide pellets and then stirred vigorously for 30 minutes. The reaction mixture was filtered over sodium sulfate, concentrated in vacuo, redissolved in methylene chloride (10 mL), dried once more over sodium sulfate, filtered, and concentrated in vacuo to afford a yellow crystalline solid, which was used in the next step without any further purification (400 mg, 100%).

Aufarbeitung

  1. customThe reaction was quenched with a few drops of water
  2. additiondiluted with diethyl ether (50 mL) and tetrahydrofuran (25 mL)
  3. additionThe reaction mixture was basified to a pH of ˜11 by the addition of potassium hydroxide pellets
  4. stirringstirred vigorously for 30 minutes
  5. filtrationThe reaction mixture was filtered over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. dissolutionredissolved in methylene chloride (10 mL)
  8. dry with materialdried once more over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customto afford a yellow crystalline solid, which
  12. customwas used in the next step without any further purification (400 mg, 100%)

Quellen und Nachweise

ORD-Eintrag
ord-8c2b4dbc37494cfb83c23da8bfe60101
Quelldatensatz
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09440976B2

Notizen zur Reaktion

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