Ethanol → 114812-34-9

HRID 1463517Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1463517
[NH:1]1[CH2:5][CH2:4][CH2:3][C@H:2]1[C:6]([NH2:8])=[O:7].[CH2:9](O)[CH3:10].C(N(CC)CC)C.C(Br)C>C1(C)C=CC=CC=1>[CH2:9]([N:1]1[CH2:5][CH2:4][CH2:3][C@H:2]1[C:6]([NH2:8])=[O:7])[CH3:10]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 6332Ethyl BromideHCID 8471TriethylamineHCID 111306L-Prolinamide

Produkt 1

HCID 10866443114812-34-9

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a solution of (S)-2-pyrrolidine carboxamide (13.2 g, 116 mmol) in ethanol (140 ml) K2CO3 (17.6 g, 128 mmol) and triethylamine (1.2 ml, 8.6 mmol) were added. The mixture was heated to 30 C. and stirred vigorously. Then ethylbromide (10.4 ml, 138 mmol) were added during 0.5 hours. After 30 hours the mixture was diluted with toluene (50 ml) and washed with water (50 ml). The organic layer was concentrated at reduced pressure. The residue was dissolved in toluene (150 ml) and washed with a small amount of aqueous sodium hydroxide, dried with magnesium sulfate, and evaporated to dryness in vacuo. Yield 10.7 g (65%).

Aufarbeitung

  1. temperatureThe mixture was heated to 30 C
  2. washwashed with water (50 ml)
  3. concentrationThe organic layer was concentrated at reduced pressure
  4. dissolutionThe residue was dissolved in toluene (150 ml)
  5. washwashed with a small amount of aqueous sodium hydroxide
  6. dry with materialdried with magnesium sulfate
  7. customevaporated to dryness in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1faed03adb3f45bebd879e17cfc1840d
Quelldatensatz
uspto-grants-1994_04
Patentnummer
US05300660

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