Chlorosulfonic acid → HCID 18541162, Verbindung

HRID 411603Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 411603
[O:1]([CH2:8][CH2:9][N:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.O(CCN1CCOCC1)C1C=CC=CC=1.[Cl:32][S:33](O)(=[O:35])=[O:34]>ClCCl>[N:10]1([CH2:9][CH2:8][O:1][C:2]2[CH:7]=[CH:6][C:5]([S:33]([Cl:32])(=[O:35])=[O:34])=[CH:4][CH:3]=2)[CH2:11][CH2:12][O:13][CH2:14][CH2:15]1

Komponenten

5

Edukt 3

HCID 24638Chlorosulfonic acid2×HCID 28409994-(2-Phenoxyethyl)morpholineHCID 6996069929488-54-8

Produkt 1

HCID 18541162HCID 18541162, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

[2-(Morpholin-4-yl)ethoxy]benzene-4-sulfonyl chloride was prepared using N-(2-phenoxyethyl) morpholine by similar reaction described above. For example, 7.2 g of N-(2-phenoxyethyl)morpholine HCl salt was resuspended in 20 ml of dichloromethane and 7 ml of chlorosulfonic acid was slowly introduced with cooling by ice-jacket. The reaction mixture was stirred at 0° C. for 2 hr, then, at room temperature overnight. Dichloromethane (350 ml) was added to the reaction mixture and excess chlorosulfonic acid was destroyed by adding icy water(about 100 g). Aqueous layer was adjusted to pH 8.5 by concentrated sodium carbonate solution with cooling by ice. Dichloromethane was dried over anhydrous magnesium sulfate and evaporated under reduced pressure to give 8.1 g of [2-(morpholin-4-yl)ethoxy]benzene-4-sulfonyl chloride. M.P. 48-50° C.

Aufarbeitung

  1. custom[2-(Morpholin-4-yl)ethoxy]benzene-4-sulfonyl chloride was prepared
  2. customby similar reaction
  3. temperaturewith cooling by ice-jacket
  4. customat room temperature
  5. customovernight
  6. customwas destroyed
  7. additionby adding icy water(about 100 g)
  8. temperaturewith cooling by ice
  9. dry with materialDichloromethane was dried over anhydrous magnesium sulfate
  10. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-dbb985ddc5d043828975100e1d40228c
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06559167B1

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