Triethylamine → HCID 13885366, Verbindung

HRID 2232020Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2232020
[F:1][S:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11](Cl)(=[O:13])=[O:12])(=[O:4])=[O:3].[NH:15]1[CH2:18][CH2:17][CH2:16]1.C(N(CC)CC)C>C(#N)C>[N:15]1([S:11]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[S:2]([F:1])(=[O:4])=[O:3])(=[O:13])=[O:12])[CH2:18][CH2:17][CH2:16]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 10422AzetidineHCID 976312-Fluorosulphonylbenzenesulphonyl chloride

Produkt 1

HCID 13885366HCID 13885366, VerbindungAusbeute 100,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

In a flask was placed 9.24 g of 2-fluorosulfonylbenzenesulfonyl chloride and 200 ml of dry acetonitrile. The resultant solution was cooled to 0° C. An addition funnel was charged with 2 g of azetidine, 4.95 ml of triethylamine and 50 ml of acetonitrile. This solution was added dropwise to the first solution. After stirring overnight the solvent was evaporated under reduced pressure. The residue was partitioned between dichloromethane and 1N hydrochloric acid. The organic layer was separated, dried and concentrated to give 9.80 g of a solid, m.p. 93° C.

Aufarbeitung

  1. customIn a flask was placed
  2. additionThis solution was added dropwise to the first solution
  3. customwas evaporated under reduced pressure
  4. customThe residue was partitioned between dichloromethane and 1N hydrochloric acid
  5. customThe organic layer was separated
  6. customdried
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-9b8977cf11df402ba2ef64eab96b2caf
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04786316

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