StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Acetic Acid → Methyl (3S,4R)-4-(2,4-difluorophenyl)-1-isopropylpyrrolidine-3-carboxylate

HRID 1992677
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1992677
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C.[CH3:19][C:20]([CH3:22])=O.[F:23][C:24]1[CH:29]=[C:28]([F:30])[CH:27]=[CH:26][C:25]=1[C@@H:31]1[CH2:35][NH:34][CH2:33][C@H:32]1[C:36]([O:38][CH3:39])=[O:37].C(=O)([O-])O.[Na+]>ClCCl.[Cl-].[Na+].O>[F:23][C:24]1[CH:29]=[C:28]([F:30])[CH:27]=[CH:26][C:25]=1[C@@H:31]1[CH2:35][N:34]([CH:20]([CH3:22])[CH3:19])[CH2:33][C@H:32]1[C:36]([O:38][CH3:39])=[O:37]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 176Acetic AcidHCID 180AcetoneHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 59130986methyl (3S,4R)-4-(2,4-difluorophenyl)pyrrolidine-3-carboxylate

Produkt 1

HCID 59130981Methyl (3S,4R)-4-(2,4-difluorophenyl)-1-isopropylpyrrolidine-3-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittel2×HCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

Sodium triacetoxyborohydride (1.32 g, 6.22 mmol) and acetic acid (235 μL, 4.14 mmol) were added to a solution of acetone (304 μL, 4.14 mmol) and methyl (3S,4R)-4-(2,4-difluorophenyl)pyrrolidine-3-carboxylate, from preparation 31 (1 g, 4.14 mmol) in dichloromethane (20 mL) at room temperature. The resulting mixture was stirred for 2 hours and diluted with dichloromethane (10 mL). Aqueous sodium hydrogen carbonate solution was added (2×20 mL) followed by brine (20 mL). The phases were separated, the organic phase was dried over magnesium sulfate, filtered and the solvent was removed in vacuo to give the crude residue. Purification of the residue by column chromatography using dichloromethane:methanol (99:1-98:2) as eluent afforded the desired product, 1.01 g (86%).

Aufarbeitung

  1. customThe phases were separated
  2. dry with materialthe organic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent was removed in vacuo
  5. customto give the crude residue
  6. customPurification of the residue by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-2e16f5cf4a8a4818b8784bfc91aa6392
Quelldatensatz
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07649002B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion