Triethylamine → HCID 13306708, Verbindung

HRID 572028Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 572028
[OH:1][CH2:2][C@H:3]1[NH:7][C:6](=[O:8])[CH2:5][CH2:4]1.C(N(CC)CC)C.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>ClCCl>[CH3:16][S:17]([O:1][CH2:2][C@@H:3]1[CH2:4][CH2:5][C:6](=[O:8])[NH:7]1)(=[O:19])=[O:18]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 643511(S)-5-(Hydroxymethyl)-2-pyrrolidinone

Produkt 1

HCID 13306708HCID 13306708, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of (5S)-5-(hydroxymethyl)pyrrolidin-2-one (1.0 g, 8.69 mmol) in dichloromethane (40 mL) at 0° C. was added triethylamine (1.816 mL, 13.03 mmol) followed by dropwise addition of methanesulfonyl chloride (0.812 mL, 10.42 mmol). The resulting mixture was stirred at room temperature for two hours, and then it was partitioned between water and dichloromethane (3×). The organic extracts were combined and dried over Na2SO4, the drying agent was removed by filtration, and the solution was concentrated in vacuo to give the title compound as a colorless, waxy solid (1.68 g, quantitative).

Aufarbeitung

  1. customit was partitioned between water and dichloromethane (3×)
  2. dry with materialdried over Na2SO4
  3. customthe drying agent was removed by filtration
  4. concentrationthe solution was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2f984cc3c8ed407b91d68c92ac6132ee
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09029361B2

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