4-Fluorobenzoic Acid → 3-(Chlorosulfonyl)-4-fluorobenzoic acid

HRID 33781

Reaktionsgleichung

Reaktionsgleichung von HRID 33781
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1>>[Cl:1][S:2]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][C:7]=1[F:6])[C:11]([OH:13])=[O:12])(=[O:5])=[O:3]

Komponenten

3

Edukt 2

HCID 99734-Fluorobenzoic AcidHCID 24638Chlorosulfonic acid

Produkt 1

HCID 39298913-(Chlorosulfonyl)-4-fluorobenzoic acid

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

Chlorosulphonic acid (100 ml, 1.5 mol) was gradually added to 4-fluorobenzoic acid (43 g, 0.307 mol) with stirring. The clear dark yellow mixture was heated to 150° C. for 24 hours. The yellow solution was cooled back to room temperature and poured onto ice with vigorous stirring. The white precipitate was filtered and pressed dry. The solid was dried overnight in a desiccator under vacuum and over activated silica (54.65 g, 75%). Mp: 116-117° C.; m/z (LC-MS, ESP), RT=4.03 min, (M−−1)=237-239 (ratio 1:3).

Aufarbeitung

  1. temperatureThe yellow solution was cooled back to room temperature
  2. additionpoured onto ice with vigorous stirring
  3. filtrationThe white precipitate was filtered
  4. custompressed dry
  5. customThe solid was dried overnight in a desiccator under vacuum and over activated silica (54.65 g, 75%)

Quellen und Nachweise

ORD-Eintrag
ord-b5bb2f4675124571b48d8ac00275062e
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07429660B2

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