Acetic Anhydride → 2-thiocyanatoethyl acetate

HRID 2078636Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2078636
[S-:1][C:2]#[N:3].[C:4]([O:7][C:8](=O)[CH3:9])(=[O:6])[CH3:5]>N1C=CC=CC=1.ClCCl>[C:4]([O:7][CH2:8][CH2:9][S:1][C:2]#[N:3])(=[O:6])[CH3:5]

Komponenten

5

Edukt 2

HCID 7918Acetic AnhydrideHCID 9322Thiocyanate

Produkt 1

HCID 2327002-thiocyanatoethyl acetate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A mixture of 2-bromoethanol (7.0 g) and potassium thiocyanate (5.4 g) in methanol (40 ml) was refluxed for 7 hours. After precipitate was filtered off, the filtrate was evaporated under reduced pressure. The residue was suspended in chloroform/methanol (5/1). The precipitate was filtered off. The filtrate was evaporated under reduced pressure to give the thiocyanate (4.4 g). To a mixture of the thiocyanate in pyridine (4.8 ml)/dichloromethane (20 ml) was added acetic anhydride (5.3 ml) in dichloromethane (5 ml) at 5° C. The mixture was stirred at room temperature for 6 hours. The precipitate was filtered off. The filtrate was washed with water, dried over sodium sulfate and evaporated under reduced pressure to give 2-thiocyanatoethyl acetate (5.6 g).

Aufarbeitung

  1. filtrationThe precipitate was filtered off
  2. washThe filtrate was washed with water
  3. dry with materialdried over sodium sulfate
  4. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f271f7cbb72c49e5987e2aedb10e3a54
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928264B2

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