Triethylsilane → 6-(2-Bromoethyl)benzothiazolone

HRID 326237

Reaktionsgleichung

Reaktionsgleichung von HRID 326237
[Br:1][CH2:2][C:3]([C:5]1[CH:14]=[CH:13][C:8]2[N:9]=[CH:10][S:11](=[O:12])[C:7]=2[CH:6]=1)=O.C([SiH](CC)CC)C>FC(F)(F)C(O)=O>[Br:1][CH2:2][CH2:3][C:5]1[CH:14]=[CH:13][C:8]2[N:9]=[CH:10][S:11](=[O:12])[C:7]=2[CH:6]=1

Komponenten

4

Edukt 2

HCID 12052TriethylsilaneHCID 1317178296-(Bromoacetyl)benzothiazolinone

Produkt 1

HCID 692279736-(2-Bromoethyl)benzothiazolone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

In a 500-cm3 ground-necked flask surmounted by a condenser, and placed in an oil bath, 40.8 g (0. 15 mol) of 6-(bromoacetyl)benzothiazolinone are dissolved in 90 cm3 of trifluoroacetic acid with magnetic stirring and while the temperature is stabilized at 60° C. 52.7 cm3 (0-33 mol) of triethylsilane are introduced dropwise via a dropping funnel. After the addition, the heating is stopped and the mixture is then left stirring vigorously for 30 hours. The reaction medium is hydrolyzed by pouring it into ice-cold water, and the precipitate obtained is drained and washed with water until the filtrate is neutral and then with hexane. The product is dried and recrystallized in absolute ethanol.

Aufarbeitung

  1. customIn a 500-cm3 ground-necked flask surmounted by a condenser
  2. customplaced in an oil bath
  3. customis stabilized at 60° C
  4. additionAfter the addition
  5. waitthe mixture is then left
  6. stirringstirring vigorously for 30 hours
  7. additionby pouring it into ice-cold water
  8. customthe precipitate obtained
  9. washwashed with water until the filtrate
  10. customThe product is dried
  11. customrecrystallized in absolute ethanol

Quellen und Nachweise

ORD-Eintrag
ord-15d2e87ca10742889d734c0af76b54a9
Quelldatensatz
uspto-grants-1993_12
Patentnummer
US05268381

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