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

Triethylamine → {1-[(1S)-1-(aminocarbonyl)propyl]-5-oxo-3-pyrrolidinyl}methyl 4-methylbenzenesulfonate

HRID 900310
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 900310
[OH:1][CH2:2][CH:3]1[CH2:7][N:6]([C@@H:8]([CH2:12][CH3:13])[C:9]([NH2:11])=[O:10])[C:5](=[O:14])[CH2:4]1.[CH2:15](N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24].N([CH2:30][CH:31]1[CH2:35]N([C@@H](CC)C(N)=O)[C:33](=O)[CH2:32]1)=[N+]=[N-]>C(Cl)Cl>[CH3:35][C:31]1[CH:30]=[CH:15][C:22]([S:23]([O:1][CH2:2][CH:3]2[CH2:4][C:5](=[O:14])[N:6]([C@H:8]([C:9]([NH2:11])=[O:10])[CH2:12][CH3:13])[CH2:7]2)(=[O:25])=[O:24])=[CH:33][CH:32]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8471Triethylamine2×HCID 31297Methanesulfonyl chloride2×HCID 60105793(2S)-2-[4-(azidomethyl)-2-oxo-1-pyrrolidinyl]butanamideHCID 60105803(2S)-2-[4-(hydroxymethyl)2-oxo-1-pyrrolidinyl]butanamide

Produkt 1

HCID 10291696{1-[(1S)-1-(aminocarbonyl)propyl]-5-oxo-3-pyrrolidinyl}methyl 4-methylbenzenesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

In a 4 l three necked flask fitted with mechanical stirrer, dropping funnel and reflux condenser under inert atmosphere, 114 g (569 mmoles, 1 eq) of (2S)-2-[4-(hydroxymethyl)-2-oxo-1-pyrrolidinyl]butanamide 6 are dissolved in 2 l of CH2Cl2 and cooled down to 0° C. 158.5 ml (115 g, 2 eq) of dry triethylamine are added in one portion, followed by dropwise addition of a solution of 66.3 ml (96.2 g, 1.5 eq) of methanesulfonyl chloride in 190 ml of CH2Cl2 over 1 hour, all the while maintaining the temperature below 4° C. After 4 hours, 7.5 ml of methanesulfonyl chloride and 15 ml of triethylamine are added and the mixture is kept overnight in the refrigerator. The mixture is filtered, the residue washed with CH2Cl2 and the combined organic phases concentrated to dryness to give 216 g of crude 37. It is purified by Prep LC in several batches (1 kg SiO2, CH2Cl2/EtOH, 100:0->96:4) to give 109 g of pure 37, 69%. Alternatively, {1-[(1S)-1-(aminocarbonyl)propyl]-5-oxo-3-pyrrolidinyl}methyl 4-methylbenzenesulfonate 31 is prepared in an analogous way. 7.2.2. Synthesis of (2S)-2-[4-(azidomethyl)-2-oxo-1-pyrrolidinyl]butanamide 32

Aufarbeitung

  1. temperatureall the while maintaining the temperature below 4° C
  2. waitthe mixture is kept overnight in the refrigerator
  3. filtrationThe mixture is filtered
  4. washthe residue washed with CH2Cl2
  5. concentrationthe combined organic phases concentrated to dryness
  6. customto give 216 g of crude 37
  7. customIt is purified by Prep LC in several batches (1 kg SiO2, CH2Cl2/EtOH, 100:0->96:4)
  8. customto give 109 g of pure 37, 69%

Quellen und Nachweise

ORD-Eintrag
ord-32340ce2e42d4563bbdaf51e8f3f23ff
Quelldatensatz
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07358276B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion