Sodium Carbonate → 2-Sulfanilamido-1,3,4-thiadiazole

HRID 1854259Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1854259
[S:1]1[CH:5]=[N:4][N:3]=[C:2]1[NH:6][S:7]([C:10]1[CH:15]=[CH:14][C:13]([NH:16]C(=O)C)=[CH:12][CH:11]=1)(=[O:9])=[O:8].C([O-])([O-])=O.[Na+].[Na+]>Cl>[NH2:16][C:13]1[CH:14]=[CH:15][C:10]([S:7]([NH:6][C:2]2[S:1][CH:5]=[N:4][N:3]=2)(=[O:9])=[O:8])=[CH:11][CH:12]=1

Komponenten

4

Edukt 2

HCID 10340Sodium CarbonateHCID 694845N-(4-(N-1,3,4-thiadiazol-2-ylsulfamoyl)phenyl)acetamide

Produkt 1

HCID 2347622-Sulfanilamido-1,3,4-thiadiazoleAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

Compound 102 (1.0 g, 3.6 mmol) was suspended in 3N HCl (10 mL) and heated to reflux for 30 min. The acidic mixture was neutralized with Na2CO3 solution. The precipitated product was collected by filtration, washed with water, and dried to give the product (450 mg, 1.8 mmol, 49%), mp 226° C. (lit2 mp 221-222° C.); 1H NMR (250 MHz, CDCl3) δ 5.95 (2, s), 6.57 (2, d, J=6.5 Hz), 7.41 (2, d, J=6.5 Hz), 8.68 (1, s), 14.03 (1, br s).

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux for 30 min
  3. filtrationThe precipitated product was collected by filtration
  4. washwashed with water
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e4a9b8136d1e4709b9384953406c9516
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08962663B2

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