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Diethyl Ether → Benzothiazole

HRID 2066446
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2066446
BrC[C:3]1[C:8]2[N:9]=[CH:10][S:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.[N-]=[N+]=[N-].[Na+].CCOCC>CN(C=O)C>[S:11]1[C:7]2[CH:6]=[CH:5][CH:4]=[CH:3][C:8]=2[N:9]=[CH:10]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 33557Sodium AzideHCID 574281094-(Bromomethyl)benzo[d]thiazole

Produkt 1

HCID 7222BenzothiazoleAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 4-Bromomethyl benzothiazole (20.4 g, 89.9 mmol) in 272 mL of dry DMF was treated with NaN3 (7.00 g, 108 mmol) at 20° C. and stirred at the same temperature for 5 min. The resulting mixture was quenched by addition of NaCl (5 g in 150 mL of H2O) at 0° C., diluted with Et2O (200 mL) and extracted with Et2O (200 mL×6). The organic phase was washed with NaCl (2 g in 100 mL of H2O) twice and brine (100 mL). The resulting solution was dried over MgSO4 and concentrated in vacuo. The residue was submitted to silica gel column chromatography with toluene:Et2O=50:3 to 50:5 as eluate to afford 4-azidemethyl benzothiazole as a colorless oil (15.5 g, 81.5 mmol, 91%). Rf=0.48 (toluene:Et2O=10:1); 1H NMR (400 MHz, CDCl3) δ 9.03 (1H, s), 7.95 (1H, d, J=7.7 Hz), 7.49 (2H, m), 5.01 (2H, s); 13C NMR (99.5 MHz, CDCl3) δ 154.2, 151.7, 134.3, 130.6, 126.0, 125.7, 122.1, 51.6.

Aufarbeitung

  1. customThe resulting mixture was quenched by addition of NaCl (5 g in 150 mL of H2O) at 0° C.
  2. additiondiluted with Et2O (200 mL)
  3. extractionextracted with Et2O (200 mL×6)
  4. washThe organic phase was washed with NaCl (2 g in 100 mL of H2O) twice
  5. dry with materialThe resulting solution was dried over MgSO4
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-cd111b4b883344cb892597e23758bf78
Quelldatensatz
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08293743B2

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