Triethylamine → HCID 13885366, Verbindung

HRID 1906347Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1906347
[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-e87d32659a4243828f00f0d3e96cd17e
Quelldatensatz
uspto-grants-1987_03
Patentnummer
US04652304

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