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Bromine → HCID 58085702, Verbindung

HRID 249722
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 249722
[C:1]([C:4]1[CH:5]=[C:6]([NH:16][C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])[CH:7]=[C:8]([S:10]([F:15])([F:14])([F:13])([F:12])[F:11])[CH:9]=1)(=[O:3])[CH3:2].[Br:23]Br>C(O)(=O)C.O>[Br:23][CH2:2][C:1]([C:4]1[CH:5]=[C:6]([NH:16][C:17](=[O:22])[C:18]([F:21])([F:19])[F:20])[CH:7]=[C:8]([S:10]([F:14])([F:15])([F:13])([F:12])[F:11])[CH:9]=1)=[O:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 24408BromineHCID 58085708HCID 58085708, Verbindung

Produkt 1

HCID 58085702HCID 58085702, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittel3×HCID 962WaterLösungsmittel

Versuchsvorschrift

N-(3-Acetyl-5-pentafluorosulfanylphenyl)-2,2,2-trifluoroacetamide (20 mg) was initially introduced dissolved in glacial acetic acid (1 ml), and bromine (9 mg) dissolved in glacial acetic acid (90 μl) was slowly added dropwise. After stirring at RT for 30 min, the mixture was warmed at 60° C. for 1 h. After cooling to RT, the glacial acetic acid was diluted with a large quantity of water and extracted three times with ethyl acetate. The combined extracts were washed with sodium hydrogencarbonate solution until acid-free, dried over magnesium sulfate, filtered and concentrated. The crude product obtained (24 mg) was employed in the next stage without further purification.

Aufarbeitung

  1. additionwas slowly added dropwise
  2. temperaturethe mixture was warmed at 60° C. for 1 h
  3. temperatureAfter cooling to RT
  4. extractionextracted three times with ethyl acetate
  5. washThe combined extracts were washed with sodium hydrogencarbonate solution until acid-free,
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-efe9cead89d5473296e50d7cb6a79c9b
Quelldatensatz
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07863269B2

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