Dimethylsulphamoyl chloride → HCID 20704038, Verbindung

HRID 904082Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 904082
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([OH:18])([C:14]([F:17])([F:16])[F:15])[C:10]([F:13])([F:12])[F:11])=[CH:5][CH:4]=1.[CH3:19][N:20]([CH3:25])[S:21](Cl)(=[O:23])=[O:22]>N1C=CC=CC=1>[F:17][C:14]([F:15])([F:16])[C:9]([C:6]1[CH:5]=[CH:4][C:3]([N:2]([CH3:1])[S:21]([N:20]([CH3:25])[CH3:19])(=[O:23])=[O:22])=[CH:8][CH:7]=1)([OH:18])[C:10]([F:12])([F:13])[F:11]

Komponenten

4

Edukt 2

HCID 83372Dimethylsulphamoyl chlorideHCID 8050151,1,1,3,3,3-Hexafluoro-2-(4-(methylamino)phenyl)propan-2-OL

Produkt 1

HCID 20704038HCID 20704038, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

To 5.4 g (20 mmole) N-methyl-4-(hexafluoro-2-hydroxy-2-propyl)aniline in 50 ml pyridine add 4.3 g (30 mmole) dimethylsulfamoyl chloride. Stir 16 hours, pour onto water, acidify and extract with Et2O. Wash with 1N NaOH, acidify the aqueous layer, and extract with Et2O. Dry, concentrate and recrystallize first from CCl4, and then from Et2O-hexane to obtain the product; m.p. 63°-65° C.

Aufarbeitung

  1. additionpour onto water
  2. extractionextract with Et2O
  3. washWash with 1N NaOH
  4. extractionextract with Et2O
  5. customDry
  6. concentrationconcentrate
  7. customrecrystallize first from CCl4
  8. customfrom Et2O-hexane to obtain the product

Quellen und Nachweise

ORD-Eintrag
ord-652893c945fb47a98e2a55df151411d4
Quelldatensatz
uspto-grants-1980_10
Patentnummer
US04230635

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